Development of Fiber Concrete

présentée par
THESE / UNIVERISTE DE BRETAGNE SUD

sous le sceau de l’Université européenne de Bretagne Riana Herlina LUMINGKEWAS
pour obtenir le titre de
DOCTEUR DE L’UNIVERISTE DE BRETAGNE SUD
Mention : Science de l’ingénieur
Ecole doctorale SICMA
Development of Materials Thèse soutenue le //2015

devant le jury composé de :
for Construction with M. Dedi PRIADI

Professeur, Universitas Indonesia / Examinateur
Low Environmental M. Irwan KATILI

Professeur, Universitas Indonesia ./ Directrice de thèse
M. Heru PURNOMO
Impact Made with Low Maître de conférences HDR, Universitas Indonesia / Co-directrice de thèse
M. Yannick MELINGE
Content of Cement and Professeur, Université de Cergy- Pontoise / Examinateur

M. TAVIO
Professeur, Institut Teknologi Surabaya / Examinateur
With Natural Fibers M. Gilles AUSIAS
Maître de conférences HDR, Université de Bretagne Sud / Directrice de thèse
M. Thibaut LECOMPTE
Maître de conférences HDR, Université de Bretagne Sud / Co-directrice de thèse
M. Arnaud PERROT
Maître de conférences HDR, Université de Bretagne Sud / Co-directrice de thèse
Development of materials for construction with low environmental Impact made with low content of cement and with natural fibers
Riana Herlina Lumingkewas 2015
ACKNOWLEDGEMENTS
The research reported in this dissertation was a part of cooperation between

Université de Bretagne Sud, UBS France and Universitas Indonesia, UI Indonesia.
I would like to express my sincere gratitude to my supervisors Assoc. Prof.
Gilles AUSIAS and Prof. Irwan KATILI, who gave me the chance to work with this
collaboration on this interesting project. I would also like to thank my co-supervisors
Assoc. Prof. Thibaut LECOMPTE, Assoc. Prof. Arnaud PERROT and Assoc. Prof.
Heru PURNOMO, who provided me an excellent source of help and support for the
present work in France and Indonesia. Without their invaluable guidance and support, this
dissertation work would have never been accomplished. They have not only been
advisors, but also mentors and friends to me. Their mentorship was and will be
paramount in providing a well-rounded experience for both the academic part of my
career and another aspect of my life.
I would like to thanks, Prof. Yannick Melinge, Prof. Tavio, and Prof. Dedi
Priadi for giving me the honor to accept being part of my thesis jury. Their careful
reading of my dissertation report and their comments were relevant and contributed to
improving the dissertation report.
I would like to thanks and appreciate for the scholarship provided by Indonesian
Government (DIKTI) during my study. As well as France Government (BGF) for the
scholarship during my study in France, that made my Ph.D. work possible. I am very
grateful to Université de Bretagne Sud (UBS), Universitas Indonesia(UI), and Institut
Teknologi Indonesia (ITI) for their continuous support my study.
I would like to thanks particularly: Prof. Sébastien LEFEVRE Directeur-
Adjoint de l‘école doctorale ED SICMA UBS. Prof. Pierre-Yves MANACH Directeur
Laboratories d'Ingenierie des Matériaux de Bretagne (LIMATB), Université de Bretagne
Sud (UBS) and Prof. Sandrine THUILLIER for their participation in the realization of
this dissertation.
I offer my sincere regards to those friends and colleagues in Laboratories
d'Ingenierie des Matériaux de Bretagne (LIMATB), Université de Bretagne Sud (UBS),
Université de Bretagne Européenne (EA 4250). Hervé Bellegou, Francoise Peresse,
Séverine Georgin, Jean Costa, Anthony Magueresse, Anthony Jegat, Pierre Tronet,
Khelifi Hamid, Thanh Hung Pham, Alice Youssef, Anaële, they help my life to be
easier in France. Moreover, also my colleagues in Universitas Indonesia, my very
heartfelt thanks go to my friends who shared much laughter, debates, ideas, but which,
above all, proved their support and understanding.
My deepest gratitude to My Parents in heaven, for their endless love and
unending encouragement and prayers to me. Last, but not least, the high words. I would
like to dedicate this dissertation to my dear husband, Prof. Sigit P Hadiwardoyo, and my
lovely children, Rietsi Arvitricia Hadiwardoyo, SE, MM; Seilendria Ardityarama
Hadiwardoyo, ST, MSc; Finno Ariandiyudha Hadiwardoyo; Graidy Arianugraha
Hadiwardoyo for their love, understanding, and support in every aspect.
(Riana Herlina Lumingkewas-Hadiwardoyo)
CONTENTS
ACKNOWLEDGEMENTS ..................................................................................................................... i
CONTENTS ........................................................................................................................................... ii
LIST OF FIGURES ............................................................................................................................... vi
LIST OF TABLES ................................................................................................................................ xv
CHAPTER.1. .......................................................................................................................................... 1
GENERAL INTRODUCTION............................................................................................................... 1
1.1. Research background .......................................................................................... 1
1.2. Research Question .............................................................................................. 4
1.3. Objective of research .......................................................................................... 4
1.4. Limitation of Research........................................................................................ 5
1.5. Contribution of Research .................................................................................... 5
1.6. Overview of Dissertation .................................................................................... 6
CHAPTER.2. .......................................................................................................................................... 8
LITERATURE REVIEW ....................................................................................................................... 8
2.1. Introduction ............................................................................................................. 8
2.2. Natural Fiber............................................................................................................ 8
2.2.1. Structure and chemical composition. ............................................................... 9
2.2.2. Physical and mechanical properties ............................................................... 11
2.2.3. Microstructure ................................................................................................ 16
2.3. Coir fibers .............................................................................................................. 17
2.3.1. Production coir fibers ..................................................................................... 17
2.3.2. Extraction of coir fibers ................................................................................. 19
2.3.3. Physical and chemical properties ................................................................... 20
2.3.4. Mechanical properties .................................................................................... 23
2.3.5. Thermal properties ......................................................................................... 24
2.3.6. Microstructure ................................................................................................ 24
2.4. Natural fiber reinforced cementitious composites. ................................................ 26
2.4.1. Rheological behavior ..................................................................................... 28
2.4.2. Physical properties ......................................................................................... 30
2.4.3. Mechanical properties .................................................................................... 30
2.4.4. Thermal properties ......................................................................................... 32
2.4.5. The fiber–matrix interface.............................................................................. 33
2.5. Extrusion of cementitious composites ................................................................... 34
2.5.1. Extrudability of cementitious materials. ........................................................ 37
2.5.2. Extrudability of fibers cementitious materials. .............................................. 38
2.6. Environmental impact ........................................................................................... 39
2.6.1. Life cycle assessment methodology ............................................................... 40
2.6.2. CO2 emissions ............................................................................................... 41
2.7. Conclusions of chapter .......................................................................................... 44
CHAPTER.3. ........................................................................................................................................ 46
RESEARCH DESIGN AND METHODOLOGY ................................................................................ 46
3.1. Introduction ........................................................................................................... 46
3.2. Flow chart of the experimental approach .............................................................. 46
3.3. Fibers ..................................................................................................................... 48
ii
3.3.1. Preparation of fibers ....................................................................................... 48
3.3.2. Water absorption ............................................................................................ 51
3.3.3. Density tests ................................................................................................... 51
3.3.4. Optical microscopy ........................................................................................ 52
3.3.5. Mechanical testing ......................................................................................... 52
3.3.6. Scanning electron microscopy ....................................................................... 54
3.3.7. Thermal gravimetric analysis ......................................................................... 56
3.4. Fiber reinforced cement mortars, at fresh state. .................................................... 57
3.4.1. Materials are tested. ....................................................................................... 57
3.4.2. Mix proportion ............................................................................................... 60
3.4.3. Mixing procedures ......................................................................................... 61
3.4.4. Rheometer tests .............................................................................................. 61
3.4.5. Screw Extrusion ............................................................................................. 63
3.4.6. Casting procedure........................................................................................... 64
3.5. Fiber reinforced mortar composites at hardened state. .......................................... 65
3.5.1. Specimens preparation ................................................................................... 65
3.5.2. Water absorption. ........................................................................................... 66
3.5.3. Density tests. .................................................................................................. 66
3.5.4. Compressive tests. .......................................................................................... 67
3.5.5. Tensile tests .................................................................................................... 68
3.5.6. Digital image correlation.............................................................................. 68
3.5.7. Microscopic observation. ............................................................................... 70
CHAPTER.4. ........................................................................................................................................ 71
PHYSICAL, MICROSTRUCTURE, THERMAL AND MECHANICAL
PERFORMANCES OF COIR FIBERS................................................................................................ 71
4.1. Introduction ........................................................................................................... 71
4.2. Physical properties................................................................................................. 72
4.2.1. Length of coir fiber ........................................................................................ 72
4.2.2. Diameter of coir fiber ..................................................................................... 73
4.2.3. Density of coir fiber ....................................................................................... 75
4.2.4. Water absorption of coir fiber ........................................................................ 76
4.3. Microstructure analysis ......................................................................................... 77
4.3.1. Surface morphological characterization ......................................................... 77
4.3.2. Energy dispersive spectroscopy analysis. ...................................................... 80
4.3.3. Fracture surfaces observations. ...................................................................... 83
4.4. Thermogravimetric analysis .................................................................................. 86
4.4.1. Residual weight .............................................................................................. 88
4.4.2. Derivative weight ........................................................................................... 89
4.4.3. Heat flow ........................................................................................................ 90
4.5. Mechanical properties ........................................................................................... 91
4.5.1. Tensile strengths............................................................................................. 91
4.5.2. Young‘s modulus ........................................................................................... 93
4.5.3. Elongation at break ........................................................................................ 94
4.7. Conclusions of chapter .......................................................................................... 96
CHAPTER.5. ........................................................................................................................................ 97
DESIGN, RHEOLOGY PROPERTIES, MICROSTRUCTURE, AND RHEOLOGY
MODEL OF PRODUCT EXTRUDED FIBER COMPOSITES .......................................................... 97
5.1. Introduction....................................................................................................... 97
5.2. Mix-Design of low cement content in mortar for extrusion .................................. 98
5.2.1. Mix design of an extrudable mortar. .............................................................. 98
5.2.2. The water content in clay mortar.................................................................. 100
iii
5.2.3. Influence water content on cement mortar. .................................................. 101
5.2.4. The formulation of an extruded fiber reinforced composites. ...................... 103
5.3. Morphologies of fresh fiber mortar composite .................................................... 107
5.4. Rheology properties of fiber mortar composite extrudability ........................... 110
5.4.1. Fiber content and fibers length on torque..................................................... 111
5.4.2. Fibers content and fibers length on yield stress. .......................................... 112
5.5. Rheology model................................................................................................... 115
5.5.1. Relative yield stress as a function of the fiber factor ................................... 116
5.5.2. The proposed rheological model to predict yield stress ............................... 119
5.5.3. Validation the rheological model. ................................................................ 121
5.6. Conclusions of chapter ........................................................................................ 122
CHAPTER.6. ...................................................................................................................................... 124

MECHANICAL PERFORMANCE, MICROSTRUCTURE, FAILURE MODE, AND
MODEL OF SCREW EXTRUDED FIBER COMPOSITES USING DESTRUCTIVE
TESTING METHOD........................................................................................................................... 124
6.1. Introduction ......................................................................................................... 124
6.2. The aspect surface of screw extrusion. ................................................................ 125
6.2.1. Surface of extruded mortar........................................................................ 125
6.2.2. Surface of extruded composites ............................................................ 126
6.2.3. Surface of mold and extrusion .................................................................. 127
6.3. Orientation fibers in screw extrusion................................................................... 127
6.3.1. Longitudinal ................................................................................................ 128
6.3.2. Transversal .................................................................................................. 129
6.4. Mechanical performance extruded composites. .................................................. 129
6.4.1. Compressive stress-strain of extruded composite ..................................... 129
6.4.2. Tensile stress-strain of extruded composite .............................................. 131
6.4.3. Stress-strain of molded and extruded sample behavior ............................... 133
6.5. Failure modes. ..................................................................................................... 135
6.5.1. Failure modes in compression ..................................................................... 135
6.5.2. Failure modes in tension ............................................................................. 138
6.6. Mechanical models ............................................................................................. 141
6.6.1. Compressive strength behavior .................................................................... 141
6.6.2. Tensile strength behavior ............................................................................. 144
6.6.3. Compressive modulus behavior ................................................................... 146
6.6.4. Tensile modulus behavior ............................................................................ 150
6.6.5. Density behavior ......................................................................................... 153
6.6.6. Strain Behavior............................................................................................ 157
6.7. The conclusion of the chapter.............................................................................. 161
CHAPTER.7. ...................................................................................................................................... 164

MICROMECHANICS, MICROSTRUCTURE, DAMAGE AND MODELS OF SCREW
EXTRUDED FIBER COMPOSITES USING NONDESTRUCTIVE TESTING
METHOD ........................................................................................................................................... 164
7.1. Introduction ......................................................................................................... 164
7.2. Mechanical characteristics of fiber composite behavior ..................................... 164
7.2.1. Compressive strength behavior .................................................................... 164
7.2.2. Tensile strength behavior ............................................................................. 166
7.3. Damage Evolution. .............................................................................................. 168
7.3.1. the compressive strength of extruded composites ....................................... 168
7.3.2. Composites extruded on tensile strength ...................................................... 171
7.4. Microstructure ................................................................................................. 174
7.4.1. Fractography ................................................................................................ 174
iv
7.4.2. Interfacial transition zone. ............................................................................ 176
7.5. Micromechanical models..................................................................................... 178
7.5.1. Micromechanical models for tensile strength. ............................................. 178
7.5.2. Micromechanical models for compressive strength .................................... 182
7.5.3. Comparison between models and experimental results ............................... 185
7.6. Conclusions of chapter ........................................................................................ 187
CHAPTER.8. ...................................................................................................................................... 189

GENERAL CONCLUSIONS AND FURTHER RESEARCH .......................................................... 189
8.1. Conclusions. ........................................................................................................ 189
8.2. Further Research.................................................................................................. 193
REFERENCES ................................................................................................................................... 195
APPENDICES .................................................................................................................................... 212

International Journal And Proceeding Published ....................................................... 212
ABSTRAK .......................................................................................................................................... 213

RESUME ............................................................................................................................................ 214
ABSTRACT ....................................................................................................................................... 215
LIST OF FIGURES
Page
Figure.2.1. Stress versus percentage strains of various fibers ............................ 14

Figure.2.2. Typical stress-strain curves for the non-wood plant fiber
bundles ............................................................................................. 14
Figure.2.3. Relationship between diameter and tensile strength of non-
wood plant fiber bundles .................................................................. 15
Figure.2.4. Relationship between diameter and Young‘s modulus of non-
wood plant fiber bundles ............................................................... 15
Figure.2.5. The SEM micrographs of the longitudinal section and cross-
sectional area of fiber strands........................................................... 16
Figure.2.6. Productivity of coconut lands in the world in Nuts/ha ..................... 19
Figure.2.7. SEM pictures: (A) raw coir fiber, (B) alkali treated coir fiber ......... 25
Figure 2.8. Newtonian and Bingham flow models ............................................. 29
Figure 2.9. General effects of concrete constituents on the Bingham
parameter .......................................................................................... 30
Figure 2.10. Evolution of the extrusion according to the ram advance for
different speeds of extrusion effort. ................................................ 36
Figure.2.11. Appearance of the surface defects according to the extrusion
speed. ............................................................................................... 36
Figure.2.12. Border field of extrusion of plastic material - no effect - speed
according ......................................................................................... 38
Figure.2.13. Global CO2 emissions per region from fossil fuel use and
cement production. .......................................................................... 42
Figure.2.14. CO2 emissions per country from fossil fuel utilization and
cement production ......................................................................... 43
Figure.3.1. The flow chart of the research design ................................................. 47

Figure.3.2. Extracted Coconut Fiber ..................................................................... 49
Figure 3.3. Coconut fibers.................................................................................... 50
Figure 3.4. Untreated coconut fibers. ................................................................... 50
Figure.3.5. Treated coir fiber ............................................................................... 50
vi
Figure 3.6. Density measurement using balances device. ................................... 52
Figure.3.7. Optical Microscopy ........................................................................... 52
Figure.3.8. Set up of the tensile test ..................................................................... 53
Figure.3.9. Preparation of specimen for the tensile test ....................................... 53
Figure.3.10. Vacuum-system ................................................................................ 55
Figure.3.11. Set up of Scanning Electron Microscope ........................................ 55
Figure.3.12. Thermogravimetric analyses device. ............................................... 56
Figure.3.13. Thermo Gravimetric Analyses (TGA) ............................................. 56
Figure.3.14. Particle size distribution of sand....................................................... 58
Figure 3.15. Coir Fibers Geometry ....................................................................... 60
Figure 3.16. Chopped Coir Fibers ......................................................................... 60
Figure. 3.17. Hobart mixer .................................................................................... 61
Figure 3.18. The Anton Paar Rheolab QC Rheometer ......................................... 63
Figure.3.19. Screw Extrusion................................................................................ 64
Figure.3.20. Cutting extruded the mortar .............................................................. 64
Figure.3.21. Cylinder sample ................................................................................ 65
Figure.3.22. Vibrating of cylinder ....................................................................... 65
Figure.3.23. Sample cylinder of test ..................................................................... 66
Figure.3.24. Cylinder Axial Compression Test .................................................... 67
Figure.3.25. Tensile test setup .............................................................................. 68
Figure.3.26. Digital Image Correlation and Testing Setup ................................... 69
Figure. 4.1. Untreated coir fiber ............................................................................ 72

Figure.4.2. Treated coir fiber ................................................................................ 72
Figure.4.3. Diameter of untreated and treated coir fiber ....................................... 73
Figure.4.4. Diameter cumulative distribution of treated coir fiber by the two-
parameter Weibull ............................................................................ 74
Figure.4.5. Diameter cumulative distribution of untreated coir fiber by the two-
parameter Weibull ............................................................................ 75
Figure.4.6. The density of untreated and treated coir fiber versus fiber length. ... 76
Figure.4.7. Water absorption of coir fibers ........................................................... 77
vii
Figure.4.8. Untreated (A) and Treated (B) of coir fibers. .................................... 78
Figure.4.9. Micro-optic of untreated (A) and treated (B) single coir fiber ........... 78
Figure.4.10. SEM micrograph of surface untreated coir fiber (A. x100; B x300;
C. x1000) and treated coir fiber (D. x100; E. x300; F. x1000). 79
Figure.4.11. The surface of treated fiber with the white dots spectrum 1 ........... 80
Figure.4.12. EDS analysis of the white dots spectrum one characteristics .......... 81
Figure.4.13. The surface of treated fiber with the white dots spectrum 2 ........... 82
Figure.4.14. EDS analysis of the white dots spectrum two characteristics ......... 82
Figure.4.15. EDS analysis of the element chemical of the white dots
characteristics ................................................................................... 83
Figure.4.16. SEM image of cross-section of a typical coir fiber at x100 ............ 84
Figure.4.17. SEM image of elementary fibers which show different lumen and
cell wall of coir fiber at x 1000. ....................................................... 85
Figure.4.18. SEM image of cross section of treated coir fiber at x500 .............. 85
Figure.4.19. The SEM micrograph of the cross section of treated coir fiber at
x500 after tensile stress ................................................................... 86
Figure 4.20 TGA curves of the heated untreated coir fibers under nitrogen
atmosphere ....................................................................................... 87
Figure 4.21 TGA curves of the heated treated coir fibers under nitrogen
atmosphere ....................................................................................... 88
Figure 4.22. TGA curves of the heated treated and untreated coir fibers under
nitrogen atmosphere ......................................................................... 88
Figure 4.23. DGA curves for the heated treated and untreated coir fibers .......... 90
Figure 4.24. TGA curves of the heated treated and untreated coir fibers under
nitrogen atmosphere ......................................................................... 91
Figure 4.25. Tensile stress vs. strain curve of the coir fiber ................................. 92
Figure.4.26. Diameter versus Tensile strength of untreated and treated coir fibers
.......................................................................................................... 93
Figure.4.27. Diameter vs. Young‘s modulus of coir fibers................................... 94
Figure.4.28. Diameter vs. Elongation at break for coir fibers .............................. 95
Figure.5.1. Water content vs. cement content in mortar for a yield stress
of 20 kPa ......................................................................................... 99
viii
Figure.5.2. The torque vs. time curves for clay mortar (K40S60)
containing different masses of water ............................................ 100
Figure.5.3. The yield stress vs. water content in clay mortar ........................... 101
Figure.5.4. The torque vs. time curves of cement mortars containg
different amount of water .............................................................. 102
Figure.5.5. The yield stress vs. water content in cement mortar ...................... 102
Figure.5.6. Torque versus time curves obtained during vane tests omix-
design C1 (yield stress of 20kPa) with a water content of
0.18. ............................................................................................... 103
Figure.5.7. Torque versus time curves obtained during vane tests mix-
design C2 (yield stress of 20kPa) ................................................. 103
Figure.5.8. Torque versus time curves obtained during vane tests mix-
design C1 (yield stress of 20kPa) with a water cotent of
0.21. ............................................................................................... 104
Figure.5.9. Surface of the extruded mortar (C1 with a water content of
0.21) ............................................................................................... 104
Figure.5.10. Torque versus time curves obtained during vane tests omix-
design C2 (yield stress of 20kPa) with a water cotent of
0.19. ............................................................................................... 105
Figure 5.11. Surface of the extruded mortar (C2 with a water content of
0.19) ............................................................................................... 105
Figure.5.12. Water content and cement content in mortar for Torque 20
µNm ............................................................................................... 106
Figure.5.13. bSurface of the extruded cement mortar ...................................... 106
Figure.5.14. Morphology of fiber reinforcedmortar composites after
mixing. ........................................................................................... 108
Figure.5.15. Morphology of fiber reinforced mortar composites, fiber
content 2% ..................................................................................... 108
Figure.5.16. Morphology of fiber reinforced mortar composites, fiber
content 3% ..................................................................................... 108
Figure.5.17. Morphology of fiber reinfoced mortar composites, fiber
content 4% ..................................................................................... 109
Figure.5.18. Microstructure adhesion of fiber out of matrix ............................ 109
Figure.5.19. Microstructure adhesion of fiber embedded in a matrix................ 110
Figure.5.20. Torque vs time for different fiber contents - fibers length of 5
mm. (a) C1 and ( b) C2................................................................. 111
Figure.5.21. Torque vs time for different fiber contents - fibers length of
10 mm. (a) C1 and (b) C2.............................................................. 112
Figure.5.22. Torque vs time for different fiber contents - fibers length of
15 mm. (a) C1 and (b) C2.............................................................. 112
ix
Figure.5.23. Yield stress vs fibers content for fibers length of 5mm .................. 113
Figure.5.24. Yield stress vs fibers content for fibers length of 10mm ................ 114
Figure.5.25. Yield stress vs fibers content for fibers length of 15mm ................ 114
Figure.5.26. Relationship between the yield stress and fibers content for
C1 .................................................................................................. 115
Figure.5.27. Relationship between the yield stress and fibers content for
C2 .................................................................................................. 115
Figure.5.28. Relative yield stress as a function of the fiber factor ..................... 118
Figure.5.32. Model versus experimental yield stress for type C1....................... 121
Figure.6.1. Aspect surface cement mortar extrudability: (a) type C1, (b)
type C2 .......................................................................................... 125
Figure.6.2. Aspect surface of cross section of cement mortar extrudability:
(a) type C1 and (b) type C2 ........................................................... 126
Figure. 6.3. Aspect surface of coir fiber cement clay mortar composites
extrudability type C2: (a) 2% fiber, (b) 3% fiber, (c) 4%
fiber. .............................................................................................. 126
Figure.6.4. Aspect surface of coir fiber cement clay mortar composites
extrudability type C1 : (a) 2% fiber, (b) 3% fiber, (c) 4%
fiber. .............................................................................................. 126
Figure.6.5. Aspect surface of coir fiber cement mortar composites
forming using: (a) Mould and (b) Extrusion ................................. 127
Figure.6.6. Direction of extrusion of fiber cement mortar composites,
Longitudinal (L) and Transversal (T). ........................................... 128
Figure.6.7. Morphology fiber cement mortar composites after extrusion,
the longitudinal direction of extrusion (L). ................................... 128
Figure.6.8. Morphology fiber cement mortar composites after extrusion,
the transversal direction of extrusion (T). ..................................... 129
Figure.6.9. Typical compressive stress-strain curves mortar and composite
with fiber length of 5 mm for extruded samples ........................... 130
Figure.6.10.Typical compressive stress-strain curves mortar and composite
with fiber length of 10 mm for extruded samples ......................... 130
Figure.6.11. Typical compressive stress-strain curves mortar and
composite with fiber length of 15 mm for extruded samples ........ 131
Figure.6.12. Typical tensile stress-strain curves mortar and composite with
length fiber 5 mm of under forming using extrusion .................. 132
length fiber 10 mm of under forming using extrusion. ............... 132
length fiber 15 mm of under forming using extrusion. ............... 133
Figure.6.15. Mortar of typical compressive stress-strain curves under
forming using mold (M) and extrusion (E) type C1 and C2 ........ 134
Figure.6.16. Mortar and composite of typical compressive stress-strain
curves under forming using mold (M) and extrusion (E) ............ 134
Figure.6.17. Compressive and tensile of stress-strain curves of mortar
under forming using mold (M) and extrusion (E) ........................ 135
Figure.6.18. Typical compression failure modes of cement mortar type C1
without fiber: (a) extruded plain mortar; (b) after static
loading. .......................................................................................... 136
Figure.6.19.Typical compression failure modes of extruded cement mortar
type C2 non fiber: (a) plain mortar; (b) after static loading. ......... 136
Figure.6.20. Photograph of failure compression of static loading, ..................... 137
Figure.6.21. Photograph of failure compression of static loading: (a)
composites4% fiber, (b) composites 3% fiber, (c) composite
2% fiber. ........................................................................................ 137
Figure.6.22. Micrograph coir fiber cement clay mortar composites, after
failure compression of static loading. ............................................ 138
Figure.6.23. Micrograph composite after failure compression of static
loading, for broken fiber. ............................................................... 138
Figur. 6.24. Typical tension failure modes under static loading: (a) cement
mortar type C1 non fiber; (b) cement mortar type C2 non
fiber. .............................................................................................. 139
Figure.6.25. Typical tension failure modes under static loading of coir
cement clay mortar composite . ..................................................... 139
Figure.6.26. Failure modes of split tensile strength: (a)composite with 2%
fiber, (b) composite 3% fiber, (c) composite 4% fiber. ................. 140
Figure.6.27. Coir fiber orientation longitudinal direction of extrusion of
coir fiber cement clay mortar composites. .................................... 140
Figure.6.28. Micrograph of CFM composite, after the tensile failure of
static loading.................................................................................. 140
Figure 6.29. Micrograph coir fiber after the tensile failure of static loading,
for broken fiber. ............................................................................. 141
xi
Figure. 6.30. Effect of fiber content on compressive stress ................................ 143
Figure. 6.31. Effect of fiber length on compressive stress .................................. 143
Figure. 6.32.Effect of fiber content on tensile stress .......................................... 145
Figure. 6.33. Effect of fiber length on tensile stress ........................................... 145
Figure. 6.34.Effect of fiber content on compressive modulus. ........................... 147
Figure. 6.35. Effect of fiber length on compressive modulus. ............................ 147
Figure. 6.36. Effect of fiber content on compressive stress and compresive
modulus for fiber length 5mm. ...................................................... 148
Figure.6.37. Effect of fiber content on compressive stress and compressive
modulus for fiber length 10mm. .................................................... 148
Figure.6.38. Effect of fiber content on compressive stress and compressive
modulus for fiber length 15mm. .................................................... 149
Figure.6.39. Effect of fiber content on compressive stress and
compressive modulus .................................................................... 149
Figure.6.40.Effect of fiber content on tensile modulus. ..................................... 151
Figure.6.41.Effect of fiber length on tensile modulus. ....................................... 151
Figure. 6.42.Effect of fiber content on tensile stress and tensile modulus
for fiber length 5mm...................................................................... 152
for fiber length 10mm.................................................................... 152
for fiber length 15mm.................................................................... 152
Figure. 6.45.Effect of fiber content on tensile stress and tensile modulus ......... 153
Figure. 6.46.Effect fiber content on density........................................................ 154
Figure. 6.47.Effect fiber length on density ......................................................... 155
Figure. 6.48.Effect of fiber content on tensile stress and density for fiber
length 5mm. ................................................................................... 155
length 10mm. ................................................................................. 156
length 15mm. ................................................................................. 156
length. ............................................................................................ 157
Figure. 6.52. Effect fiber content on strain ......................................................... 158
Figure. 6.53.Effect fiber length on strain ............................................................ 159
Figure. 6.54.Effect of fiber content on tensile stress and strain for fiber
length 5mm. ................................................................................... 159
xii
length 10mm. ................................................................................. 160
length 15mm. ................................................................................. 160
length ............................................................................................. 161
Figure. 7.1. Typical compressive stress – strain curves of cement mortar

using MTS and DIC ...................................................................... 165
Figure. 7.2. Typical compressive stress – strain curves of CFM composite
using MTS and DIC ...................................................................... 165
Figure. 7.3. Typical compressive stress – strain curves of CFM composite ...... 166
Figure. 7.4. Typical split tensile stress – strain curves of cement mortar
using MTS and DIC ...................................................................... 166
Figure. 7.5. Typical split tensile stress – strain curves of CFCM composite
using MTS and DIC ...................................................................... 167
Figure. 7.6. Typical split tensile stress – strain curves of CFCM composite
using MTS and DIC ...................................................................... 167
Figure. 7.7. Evolution of apparent normal strain during the compression at
the elastic region for CFM composite. ......................................... 169
Figure. 7.8. Evolution of apparent normal strain during the compression
during inelasticitic phase for CFM composite. ............................ 169
Figure. 7.9. Evolution of apparent normal strain at selected points during the
compression at inelastic after peak load for CFM composite. ...... 170
Figure. 7.10. Evolution of apparent normal strain at selected points during
the compression at failure for CFM composite ............................ 170
Figure. 7.11. Evolution of apparent average strain during the splitting
tension static loading at elastic for CFM composite. .................... 171
Figure. 7.12. Evolution of apparent average strain during the splitting
tension at peak load for CFM composite....................................... 172
Figure. 7.13. Evolution of apparent normal strain during the splitting
tension at plastic for CFM composite........................................... 173
Figure.7.14. Fracture surface under static loading on splitting tensile of
extruded CFM composite of SEM micrograph (50x
magnification). .............................................................................. 174
xiii
Figure.7.15. SEM micrograph (200x magnification) of the fracture surface
under static loading of extruded CFM composite ........................ 175
under static loading of extruded CFM composite ........................ 175
Figure.7.17. SEM micrograph (500x magnification) of the fiber fracture
under static loading of extruded CFM composite ......................... 176
Figure.7.18. SEM micrograph (500x magnifications) of the fracture surface
of CFM composite after static loading. ........................................ 177
Figure.7.19. SEM micrograph (500x magnifications) of the fracture surface
of CFM composite after static loading. ........................................ 177
Figure. 7.20. The tensile strength versus fiber volume fraction. ........................ 179
Figure. 7.21. Relative tensile strength as a function of the fiber factor for
modification the model predictions. .............................................. 181
Figure. 7.22. The compressive strength versus fiber volume fraction. ............... 183
Figure. 7.23. Relative compressive strength versus the fiber factor for
modification the model predictions. .............................................. 184
Figure. 7.24. Model versus experimental tensile strength for the CFM
composite....................................................................................... 186
Figure. 7.25. Model versus experimental compressive strength for the CFM
composite....................................................................................... 187
xiv
LIST OF TABLES
Page
Table.2.1 Chemical composition of some natural fibers ...................................... 10

Table.2.2 Physical-mechanical properties of natural fiber ................................... 11
Table.2.3 The equilibrium moisture content of natural fiber. ............................... 12
Table.2.4 Properties of natural and synthetic fibers.............................................. 13
Table.2.5 The physical properties of coir fibers. .................................................. 22
Table.2.6 Mechanical properties of coir fibers. ................................................... 23
Table.2.7 The chemical properties of coir fibers. ................................................ 25
Table 3.1 Chemical composition of cement.......................................................... 57

Table 3.2 Chemical Composition of Kaolin ......................................................... 59
Table 3.3 Characteristics of CHRYSO Fluid Optima 206 .................................... 59
Table 4.1 Chemical composition of Coir Fibers at Spectrum one by EDS ......... 81
Table 4.2 Chemical composition of Coir Fibers at Spectrum two by EDS .......... 82
Table 4.3 Thermogravimetric results for coir fibers ............................................. 87
Table 4.4 Mechanical properties of treated and untreated coir fibers .................. 95
Table.5.1. Mixture proportions of cement, clay, and sand.................................... 99

Table 5.2. Mix formulation of the coir fiber-reinforced fresh cement
mortar for extrusion. .......................................................................................... 106
Table.5.3. Fitting parameters values for the tested materials ............................. 113
Table.5.4. Parameter value of the yield stress model.......................................... 117
Table.5.5. Parameter value of modification the yield stress model .................... 119
Table.5.6. Parameter value of modification the yield stress model .................... 121
Table.6.1. Fitting parameters values of the compressive stress versus fiber

content for the tested materials ........................................................ 142
Table.6.2. Fitting parameters values of the tensile stress versus. Fiber
Table.6.3. Fitting parameters values of the compressive modulus versus
fiber content for the tested materials................................................ 146
xv
Table.6.4. Fitting parameters values of the tensile modulus versus Fiber
Table.6.5. Fitting parameters values of the density versus fiber content for
the tested materials........................................................................... 154
Table.6.6. Fitting parameters values of the tensile strain versus fiber
Table.7.1. Comparison tensile strength of fiber composite properties

obtained from experiment and analytical model.............................. 185
Table.7.2. Comparison compressive strength of fiber composite properties
obtained from experiment and analytical model.............................. 186
xvi
CHAPTER.1.
GENERAL INTRODUCTION
1.1. Research background
Recently, researchers are extremely focused toward the global warming.

Environmental damage currently is a major concern for people. The study and design of
materials now are more geared toward preventing environmental damage. According to
CDIAC, the global production of cement contributed about 3.4% of the total carbon
dioxide (CO2) into the earth‘s atmosphere in 2003 [1]. Now represent 4.9% of total
CO2 [2]. Furthermore, the global emissions of CO2, the main cause of global warming
increased by 3% in 2011.[3]. In total, cement production accounts for roughly 9.5% of
global CO2 emissions in 2013. According to estimates by USGS (2014), cement
production increased in 2013 in most countries among which Indonesia, Iran, the
Russian Federation, Turkey and Vietnam by 5% to 10%[Olivier et al, 2014].
In the construction industry, a major component of the common materials such as steel
or cement comes from natural resources and requires much energy. Cement production
continues increased along with the increasing demand for the construction sector.
Therefore, the construction industry handles the depletion of a large number of
resources that are not renewable. This activity generates millions of tons of mineral
waste and millions of tons of carbon dioxide emissions. From the total greenhouse
gasses emitted by this sector, half is directly generated from the transportation,
manufacturing and use of materials in the construction phase [4].
The motivates researchers to develop alternative materials to reduce the amount of CO2
emissions and other toxic gasses that released into the environment. Use of
supplementary cementitious materials or valorization of local raw materials such as soils
is common options to limit environmental impacts of building materials. It is also
interesting to limit the steel reinforcement in concrete by adding bio-based fibers that
are locally available.
Use of natural fibers in cementitious composites is an alternative in

construction materials that can reduce the price, energy cost, and environmental
impact. Natural fibers are renewable and sustainable resources. It can found in a large
amount worldwide including in Indonesia. For example, the fiber of the coconut husk
is now wasted and has not been widely used as composite materials in civil
engineering. Coconut husk constituted of 30 wt. % coir fiber and of 70 wt. % pith [Jan
et al., 2004] [5], [Rodrígueza et al., 2011]. Also, coconut husk is another significant
source of cellulose. Cellulose is a classic example where the reinforcing elements and
deposited in a continuous manner. The coir fiber is natural fiber extracted from
coconut husk.
Currently in Indonesia use coir fiber limited to the results of the housing industry that
produces equipment household appliances such as doormats, brushes, vases of plants,
ropes, and textiles. There is still much waste from coconut copra industry as raw
material that mostly exported and not used optimally. Indonesia is one of the countries
with the largest potential of coconut natural resources in the world. About 87% of
coconuts lands located in the countries member of the Asian and Pacific Coconut
Community (APCC). The coconut acreage is Indonesia 32.4% and the Philippines
27.5% in the world [CAPPI, 2008].
It is worth to note that coir fiber presents ductile properties [Munawar SS et al., 2007].
Utilization of coir fiber into cementitious matrices is very suitable for earthquake-
resistant construction materials. Therefore, fiber reinforced cementitious composites
are fascinating for Indonesia, which located in an area with risk of intense earthquakes.
That surrounded by the three Indo - Australian, Eurasian and Pacific tectonic plates
where colliding can produce heaps of energy).
A study of the properties of coir fiber still limited to the countries of India, Brazil,
Malaysia, and Vietnam. [Kulkarni et al. 1981], [Satyanarayana. KG et al. 1982],
[Noguera P et al. 2003], [Munawar SS et al, 2007], [MM Rahman and MA Khan,
2007], [Jústiz-Smith CA et al, 2008], [Defoirdt N et al, 2010], [Muensri P et al, 2011],
[Ezekiela N et al, 2011], [Saw SK et al, 2011].
The material ingredients of the cementitious composite are similar to that of

fiber reinforced concrete, including cement, sand, water, fiber, and a few chemical
additives. The mixing procedure of cementitious composites is similar to that
employed for the normal concrete.
Making cementitious composites reinforced with natural fibers represent one way of
recycling waste that is of economic interest for developing countries. The cementitious
composite is a material with exciting potential. The price of the material could be 30%
cheaper than standard construction materials, and the mechanical properties of
cementitious reinforced composites can equal conventional building materials.
Moreover, conventional cement products are characterized by a brittle behavior, with
low tensile strength [Balaguru & Shah, 1992], [Kuder & Shah, 2010]. Hence, fibers
incorporated into cement matrix is likely to overcome this weakness, producing
materials with increased tensile strength, ductility, therefore, improved durability
(cracks limitation). Natural fiber reinforcement has good effects on fracture toughness
behavior, durability, environmental-induced damage and aging [Savastano Jr. et al.,
2003], [Tolêdo Filho et al., 2003].
The incorporation of such natural fibers as cement and/or earth-based materials

offers significant potential for the development of low-cost and local construction
materials for affordable housing. However, there are significant challenges that must
overcome before natural fibers can optimally incorporated into building materials. In
the field of construction materials, the industry can take part in creating and
manufacturing environmentally in a friendly building materials made from local
environmental waste and natural raw materials. It can lead to useful material for
developing countries. Therefore, to build with local materials reinforced with natural
fibers is one way to achieve sustainable development. Hence, the need for sustainable,
energy efficient construction materials has oriented extensive research on alternative
materials that can reduce the cost and environmental impact of building processes. In
either case, it reduces CO2 emissions by a lower cement proportion in concrete mixes.
In this work, studied coir fiber reinforced mixes of sand, clay, and cement are
considered cement stabilized soil to design extruded. It has been shown, that for mixes
containing more clay than cement, mechanical strength can be close to common
concrete blocks for housing [Khelifi et al. 2012].
Processing can substantially influence fiber dispersion and orientation, material

compactness, quality of the composite performance and cost of production. The
relationship between processing and composite performance is of great importance and
relatively little studied. Extrusion usually used for the forming process of food,
fertilizers, pharmaceuticals, clay, polymers, and metal can also use in cement materials
processing. It is an efficient forming process that induces high productivity and
reduced void content. Extrusion should be a valuable method to decrease the porosity
and improve mechanical strength; these are being principal characteristics of building
materials [Qian et al. 2003], [Perrot et al. 2009a].
However, use of extrusion of cement-based construction materials is still very limited.
Precast industries are interested in extrusion. Because it is a continuous process that
allows for the production of high-resistance engineered cementitious composites
[Peled & Shah, 2003], [Qian et al. 2003], [Perrot et al. 2009b]. Also, the precast
concrete plant is one solution to reducing air content by compacting concrete mixes by
pressure and vibration. It is crucial because it well known that the concrete resistance
directly linked to porosity [De Larrard & Sedran, 2002].
The cost of extruded fiber reinforced cementitious composites were significantly
reduced using alternate clay binders [Kuder & Shah, 2010]. Availability of new
building materials ready to use is still extremely limited. Extrusion use for the
production of construction materials in civil engineering is limited. On the other hand,
these tools can accelerate the productivity of the forming process. There are still
obstacles to density, mechanical strength performance, fiber-matrix adhesion and
surface appearance. However, the extrusion of cement based materials seems to be
very promising in the scope of high the mechanical performance precast concrete.
Overview of the state of the art in natural fiber cement-based composites research
highlights the need to develop alternative and sustainable new materials, using local,
energy-efficient, low-cost materials with low environmental impact. Many attempts to
develop locally optimized materials presented in the literature. However, very limited
data on the rheology, the mechanical and micromechanical properties of coir fiber
reinforced cementitious composites shown. The research approach has been carried
out, on low cement content stabilized soils (reducing emissions associated with cement
production and material transportation) and reinforced with coir fiber. Furthermore, the
coir fiber cementitious composites are processed using extrusion to limit the material
porosity. This research starts with the preparation and the performances of the coir
fiber. Then the design, processing, the performances and microstructural analysis of
the composites are presented. The physical structures, mechanical, thermal and
morphological characteristics of coir fibers studied. Mix design, rheological behavior,
extrusion, and mechanical characteristics of the coir fiber reinforced cementitious
composites are studied and propose rheology and micromechanical model.
1.2. Research Question
Currently, developments of new building material products focused on

environmental issues. How to develop new materials for industry construction with the
low environmental impact made with a low content of cement, and coir fibers using
extrusion?
This study will answer some of the new challenges and find solutions for the following
response:
1. How to improve the characteristic of coir fiber to reinforce cement based
materials?
2. How to determine formulations of productivity extrudate of coir fiber reinforced
cementitious composite?
3. What is the rheology model of the coir fiber reinforced cementitious composite?
4. What is the mechanical model of the coir fiber reinforced cementitious
composite of extrusion products?
5. What is the micromechanical model of the coir fiber cementitious composites of
extrusion products?
1.3. Objective of research
The goals of this research are to develop new environmentally friendly materials
for construction made with local raw and renewable materials such as natural fiber. To
be used for industry, these raw materials must be optimized and well characterized. All
the components studied must add into the mix at the optimized content.
Screw Extrusion will process materials and samples characterized using
Scanning Electronic Microscope (SEM), mechanical test using destructive testing,
Mechanical Testing System (MTS) and non-destructive testing Digital Image
Correlation (DIC). Coir fiber studied the physical structure, mechanical, and
microstructure. Fiber cementitious composite materials studied formulation, rheological
model, fabrication process, mechanical characteristics, microstructure, and
micromechanical model.
The outputs are to obtain:
1. The physical, mechanical, microstructure and thermal properties of coconut/coir
fiber with and without treatment.
2. The formulation of extrudate coir fibers reinforced cementitious composites.
3. The rheology model of the extrudate coir fiber reinforced cementitious
composite.
4. The mechanical behaviour and models of screw extruded of the coir fiber
reinforced cementitious composite.
5. The micromechanical model of screw extruded of the coir fiber reinforced
cementitious composites.
The long-term goal of this research is to produce new green building materials with low
cement content and high amount of local raw materials. Such as clay, sand, and
reinforced coir fibers on concrete technology for industry construction.
1.4. Limitation of Research.
Based on the above background, there is an urgency to develop new building

materials that are environmentally friendly. The use of local materials and natural
materials can replace environmentally harmful materials. New building materials and
renewable energy will reduce harmful emissions. The exploitation of the abundant
natural resources will drive the growth of the green building materials industry. This
work aims to focus on rheology, mechanical and micromechanical of new low cement
content materials reinforced with coconut/coir fiber and formed by extrusion.
1.5. Contribution of Research
The aim is to contribute to the field of civil engineering and materials science by
developing and creating environmental friendly building materials. The incorporation of
natural fibers with cement and basic materials of the Earth offers significant potential
for the development of cheap construction materials for affordable housing. Generate
new materials that applied to increase the production of readymade materials in the
construction industry. Developing local materials and waste natural fiber materials,
giving added value to agriculture, accelerating the development of environmentally
friendly building materials industry and the promotion of social economy are long-term
goals.
Also, based on the results of state of the art, advances these researchers are:
1. The characteristics of the coir fiber.
2. The method of assessing formulation of mix design for extrusion of the fiber
cementitious composite materials.
3. The rheology models for prediction yield stress of the fiber reinforced
cementitious composite.
4. The macro-mechanical model for prediction tensile strength and compressive
strength of extruded of the fiber reinforced cementitious composite.
5. The micromechanical models prediction tensile strength and compressive
strength of extruded of the fiber reinforced cementitious composite.
1.6. Overview of Dissertation
This dissertation is divided into eight chapters, as follows:
The first chapter contains an introduction describing the background and

presents recent topics and focus natural fiber cementitious composite on the concrete
technology of building materials for industry construction. Then the most current issues
that need to be solved are listed. Those issues orient our work from start to end.
The second chapter consists of a literature review, including the state of the art
of current research on the performance of fiber-reinforced cement-stabilized soils. Use
of natural fibers of coconut on building materials also investigated. Then, the review on
the extrusion of cement-based materials is done. To conclude, this chapter reviews the
issue of environmental impacts of building materials.
In the third chapter, the research methodology to achieve the research objectives
is presented. It contains a flow chart of research and implementation of experiments on
coir fibers, and coir fiber reinforced cementitious composites. Studied materials are
listed. Then, the experimental devices and protocols used to obtain the physical,
mechanical, thermal and microstructural properties are presented.
In the fourth chapter, an analysis of the performance of natural fibers from

coconut husks is performed from experimental observations and measurements. A
review conducted on the physical, mechanical, thermal, and microstructure properties of
coir fibers. Deeper observations are carried out by the influence of fiber length and
diameter of the fibers in its use as reinforced concrete.
The fifth chapter presents the composition and formulation of coir fiber
reinforced cement stabilized soil composites designed for extrusion. The influence of
the fiber content and aspect ratio on the fiber composites rheological properties and
rheology model were assessed to keep an extrudate material.
The sixth chapter presents the analysis of the experimental results of mechanical
tests performed on fiber reinforced cementitious composite materials processed by
screw extrusion. The effect of fiber length and fiber content on the material properties is
a highlight. Similarly, the processing (extrusion and molding) influence on the material
mechanical and physical properties are also studied.
The seventh chapter consists in the development of a micromechanical model

that describes the fiber-reinforced ductile cementitious composite behavior. Then, the
evolution of damage is observation. The modeling used to predict the evolution of
micromechanical is compare to experimental data provided using destructive method by
mechanical testing system and non-destructive method by digital image correlation
Finally, in the eighth chapter, the conclusions of the research and the future work
that needs are presented.
CHAPTER.2.
LITERATURE REVIEW
2.1. Introduction
The literature review and state of the art in this chapter aim to provide a
comprehensive and detailed overview of the results of recent research conducted
on environmentally friendly building materials.
This state of the art on construction materials focused on the properties

and performance characteristics of natural fibers cement, clay and fiber
cementitious composite materials. Also mix design and method of extrusion
processes for fiber reinforced cement-based composites is studied.
The mechanical performances of such composites studied at micro and

macro scales. Finally, the environmental impacts of the cement-based fiber
reinforced composites investigated, and the life cycle analysis method presented.
2.2. Natural Fiber
Natural fibers can obtain from natural resources such as plants (vegetable,
leaves and wood), animals, and geological processes. There are six basic types of
natural plant fibers. They classified as follows: 1. bast fibers (jute, flax, hemp,
ramie and kenaf), 2. leaf fibers (abaca, sisal and pineapple), 3. seed fibers (coir
and cotton), 4. core fibers (kenaf, and jute, reed fibers (wheat, corn and rice), and
all other types (wood and roots) [Faruk 2012].
Natural fibers represent a renewable resource that is available almost all

over the world [Brandt 2008]. Some of the most popular natural fiber that often
used are flax, hemp, jute, sisal, hemp, and kenaf fibers. They have been
extensively studied and used in different applications. Nowadays, abaca,
pineapple leaf, coir, oil palm, bagasse, and rice husk fibers are gaining interest
and importance to both researchers and industrial applications.
This focus is due to their properties and availability. It should mention that
there are also shortcomings: lack of consistency of fiber qualities, and conditions
of the processing; high levels of variability in fiber properties related to the
location and time of harvest; sensitivity to moisture, and UV radiation. A multi-
step manufacturing process is required to produce high-quality natural fibers,
which contributes to the cost of high-performance natural fibers as well as, the
improved mechanical properties of the composites.
Furthermore, due to cancer health risks [Azuma 2009], it is now forbidden

to cementitious product products containing silicates fiber (asbestos). Researchers
used natural fibers as an alternative source of steel and/or artificial fibers to used
in cement- based composites (cement paste, mortar, and concrete) to improve the
mechanical behavior. Among some emerging natural fibers: coir, sisal, jute, ramie
bast, pineapple leaf, bamboo, palm, banana, hemp, flax, cotton, and sugarcane are
targeted to used as reinforcement in engineered cementitious composites.
[Ramakrishna 2005; Li et al., 2007; Asasutjarita 2007; Toledo Filho 2005;
Munawar 2007; Rao 2007; Li 2006; Fernandez 2002; Reis 2006; Corradini 2006].
Natural fiber reinforced cementitious composites can use for many civil
engineering applications. Examples including roofing tiles [Agopyan 2005],
corrugated slabs [Paramasivam 1984], simple slab panels [Ramakrishna, 2005],
boards [Li 2007]; [Asasutjarita 2007]; and mortar [Toledo Filho 2005] are
reported in the literature.
2.2.1. Structure and chemical composition.
The principal components of the fiber cell walls are cellulose,

hemicellulose and lignin with pectin typically considered being the primary
binder. Cellulose is a polymer containing glucose units. It is a strong, linear
(crystalline) molecule with no branching. Cellulose has good resistance to
hydrolysis although chemical and solution treatments will degrade it to some
extent. [Heinze, 2005]. Hemicellulose is a polysaccharide polymer that consists of
low molecular weight, copolymer glucose, mannose, glucuronic acid, arabinose,
and xylose. Besides, it presents in the form of random, amorphous structure with a
small force branching. Dilute acid or base hydrolyzes the hemicellulose. This
enzyme is commercially important because they open the bound structure of
cellulosic materials [Summerscales 2010].
Lignin is an amorphous and heterogeneous mixture of polymer and

monomer aromatic phenyl-propane [John 2005] [Mohanty 2000]. The lignin is
formed by removing water from the sugar (mainly xylose) to create aromatic
structures. Lignifications occur in the mature plant. Lignin becomes more rigid,
far from the surface of the lumen, and creates a porous area that maintains the
strength of the walls and helps to transport water. Lignin is not sensitive to
microorganisms as their aromatic rings are resistant to anaerobic processes while
the aerobic breakdown of lignin is very slow. [Summerscales 2010].
Table 2.1 shows the average amount of chemical constituents for a broad
range of fiber types. The important structural component of nearly all green plant
cell walls is cellulose, especially on many natural fibers.
Climatic conditions, age and degradation process influence not only the
structure of fibers but also the chemical composition. Water is an important
chemical component of a living tree. However, on a dry basis, all plant cell walls
consist mainly of sugar-based polymers (cellulose, hemicellulose) that combined
with lignin with a lesser amount of extractives, protein, starch and inorganics. The
chemical components distributed throughout the cell wall, which are composed of
primary and secondary wall layers.
Table 2.1 Chemical composition of some natural fibers
Cellulose Hemicellulose Lignin Waxes

Fiber
(wt. %) (wt. %) (wt. %) (wt. %)
Bagasse 55.2 16.8 25.3 –

Bamboo 26–43 30 21–31 –
Flax 71 18.6–20.6 2.2 1.5
Kenaf 72 20.3 9 –
Jute 61–71 14–20 12–13 0.5
Hemp 68 15 10 0.8
Ramie 68.6–76.2 13–16 0.6–0.7 0.3
Abaca 56–63 20–25 7–9 3
Sisal 65 12 9.9 2
Coir 32–43 0.15–0.25 40–45 –
Oil palm 65 – 29 –
Pineapple 81 – 12.7 –
Curaua 73.6 9.9 7.5 –
Wheat straw 38–45 15–31 12–20 –
Rice husk 35–45 19–25 20 14–17

Rice straw 41–57 33 8–19 8–38
Source: [Faruk 2012]. It has been reprocessed.
The chemical composition varies from one fiber type to another, and
within different parts of the same plant. It also varies in plants from various
geographical regions, ages, and climate and soil conditions. The chemical
properties are influenced by the fiber growth time (days after planting), the
botanical classification of fiber and the stalk height. The chemical composition
10
can also vary within the same part of a plant. Both the root and stalk core have a
higher lignin content than that of the fibers.
2.2.2. Physical and mechanical properties
The natural fibers properties differ in all cited works because of the
differences in the fiber structure due to the overall environment conditions during
growth and stock but also due to different testing methods. However, to expand
the use of natural fibers in composites and improved their performance, it is
essential to know fiber characteristics.
Many factors can influence mechanical properties of natural fibers. First, it

is required to know if the sample consists of fiber bundles or ultimate fiber tested.
Table.2.2 presents the important physical-mechanical properties of commonly
used natural fibers collected by different authors [Faruk 2012], [Hattallia 2002],
[Hoareau 2004].
Table 2.2 Physical-mechanical properties of natural fiber
Young‘s Elongation at
Tensile strength Density
Fiber modulus break
(MPa)
(GPa) (%) (g/cm3)
Abaca 400 12 3–10 1.5

Bagasse 290 17 – 1.25
Bamboo 140–230 11–17 – 0.6–1.1
Flax 345–1035 27.6 2.7–3.2 1.5
Hemp 690 70 1.6 1.48
Jute 393–773 26.5 1.5–1.8 1.3
Kenaf 930 53 1.6 –
Sisal 511–635 9.4–22 2.0–2.5 1.5
Ramie 560 24.5 2.5 1.5
Oil palm 248 3.2 25 0.7–1.55
Pineapple 400–627 1.44 14.5 0.8–1.6
Coir 175 4–6 30 1.2

Curaua 500–1150 11.8 3.7–4.3 1.4
Source: [Faruk 2012]. Has been reprocessed
11
The physical properties of each natural fiber are critical and include the
fiber dimensions, defects, strengths, and structure. It is crucial to estimate physical
properties of each natural fiber to optimize its efficiency in a given composite.
Fiber dimensions, defects, strength, variability, crystallinity, and structure must be
taken into consideration. Moreover, the hydrophilic nature of natural fibers
influences the mechanical properties. The moisture content at a given relative
humidity has a high effect on the performance of a composite made of natural
fibers. The equilibrium moisture content of different natural fibers at 65%
relative humidity and 21oC [Rowell, 2008] given in Table 2.3.
Natural fibers have high tensile strength, comparing to they are the
relatively low modulus of elasticity (Table 2.4). Even though, their tensile
performance can stand in a favorable manner with synthetic ones. The
disadvantages of using natural fibers are that they have a high variation in their
properties that could lead to unpredictable concrete properties [Li 2006],
[Pacheco, 2011].
Table 2.3 The equilibrium moisture content of natural fiber.
Fiber Moisture Content (%)

Sisal 11
Hemp 9
Jute 12
Flax 7
Abaca 15
Ramie 9
Pineapple 13
Coir 10
Bagasse 8.8
Bamboo 8.9
Source: [Rowell 2008]. Has been reprocessed
To improve the performance of fiber reinforced cementitious composite, it

is possible to treat the fibers industrially before their incorporation into the matrix.
For example to the treatment fiber that improves the adhesion of fiber cement
matrix and also resistance to alkali attack is pulping [Savastano, 2003b]. The
latest research results provide results that fibers treatment show an improvement
in the properties of the fibers, the better rheological behavior of the cement
12
mixtures, and an increase of the mechanical strength of the composites, [Sawsen
et al., 2015]. It is also important to consider the effect of treatment on the fracture
toughness, durability, environmental-induced damage and aging of both the fiber
and the composite [Savastano, 2003a; Tolêdo Filho, 2003].
The correlation between some mechanical properties of natural fibers is

shown in Figure 2.1[Rao 2007] and Figure 2.2. [Munawar 2007]. These figures
show the stress-strain relationship for different fibers. It appears that the coir fiber
behavior is very different in both cases. It highlights the dispersion of such natural
fibers properties. Emphasis should be made to develop typical curves, not only for
a stress-strain relationship but also for other relationships. The variation of tensile
strength and Young's modulus with fiber diameter is shown in Figure 2.3 and
Figure 2.4, respectively. It can be observed that both decreases when the fiber
diameter increase.
Table 2.4 Properties of natural and synthetic fibers
Properties Specific Water Tensile Modulus of

gravity absorption strength elasticity
(kg/m3) (%) (MPa) (GPa)
Sisal 1370 110 347–378 15.2
Coconut 1177 93.8 95–118 2.8
Bamboo 1158 145 73–505 10–40
Hemp 1500 85–105 900 34

Caesar weed 1409 182 300–500 10–40
Banana 1031 407 384 20–51

Piassava palm 1054 34–108 143 5.6
Date palm 1300–1450 60–84 70–170 2.5–4
Polypropylene 913 – 250 2.0
PVA F45 1300 – 900 23
Source: [Pacheco 2011]. Has been reprocessed
13
Figure 2.1. Stress versus percentage strains of various fibers
[Rao 2007]
Figure 2.2. Typical stress-strain curves for the non-wood plant fiber bundles
[Munawar 2007]. (Note: RB, Ramie bast fiber; PL, pineapple leaf
fiber; KB, kenaf bast fiber; SaL, Sansevieria leaf fiber; CH, coconut
husk fiber; AL, abaca leaf fiber; SiL, sisal leaf fiber).
14
Figure.2.3. Relationship between diameter and tensile strength of non-wood
plant fiber bundles
Source: [Munawar 2007]
(Note: RB, Ramie bast fiber; PL, pineapple leaf fiber; KB, kenaf bast fiber;
SaL, Sansevieria leaf fiber; CH, coconut husk fiber; AL, abaca leaf fiber;
SiL, sisal leaf fiber),
Figure.2.4. Relationship between diameter and Young’s modulus of non-wood

plant fiber bundles
Source: [Munawar 2007]
(Note: RB, Ramie bast fiber; PL, pineapple leaf fiber; KB, kenaf bast fiber;
SaL, Sansevieria leaf fiber; CH, coconut husk fiber; AL, abaca leaf fiber;
SiL, sisal leaf fiber)
15
Munawar et al. characterized the morphological, physical and mechanical
properties of the non-wood plant fiber bundles (ramie, pineapple, kenaf, abaca,
sisal and coconut fiber) [Munawar 2007]. The larger the diameter of the fiber
bundles is the lesser will be the density, tensile strength, and the Young‘s
modulus.
2.2.3. Microstructure
Micrographs of fibers along the longitudinal axis showed residue on the
surfaces of the fibers [Justiz-Smith 2008]. In the case of bagasse, the residue was
mostly pith. From the microstructure of the vertical cross-sectional area
(Figure.2.5), it is observed that the single strand of the coconut fiber had a hollow
section. It suggests that the ‗single‘ strand is a series of microfibers, called a fiber
bundle.
Figure.2.5. The SEM micrographs of the longitudinal section and cross-

sectional area of fiber strands.
Source: [Jústiz-Smith 2008]
16
2.3. Coir fibers
In the recent past, coir was considered as a low-quality, low-value natural

fiber that can be used for spinning of yarn, cordage, door mats, matting, carpets,
rugs, brushes, and brooms. Even though, man-made synthetic fibers have taken
over the market for natural fibers. Natural fibers have some advantages over
synthetics fibers as they possess properties that cannot be a match or copied
easily. The current trends in enhanced utilization of ecologically friendly bio-
products have paved the way for more diversified applications for coir and value-
added products, providing greater potential for improving the rural economy in
major coir producing countries. Coir is an eco-friendly, natural, biodegradable,
durable, renewable, low-cost and sustainable product.
Coir is a versatile, non-abrasive, porous, hygroscopic, viscoelastic,

biodegradable, combustible and compostable natural product. Compared with
other natural fibers, coir fiber bundles have medium strength but interesting
elongation properties, which makes them attractive for certain technical
applications.
Coir husk fibers are located between the husk and the outer shell of the
coconut. The coconut demand mainly determined coir production. The coconut
husks are available in abundant quantities. It implies that coir producers can adjust
relatively rapidly to market conditions. It can be noted that the coir fibers are also
commercially available at relatively high cost when prepared for special purposes
like brushes, mats, and pedestal seats. This cost can be reduced if fibers are
mechanically processed at large scales. Until now there has been no commercial
product that provides fiber-based uniform size and fiber size below 100 mm. The
numbers of coconuts harvested annually in the world are about 55 billion, but only
15% of the husk fibers are recovered for use [Wang 2009]. Most husks are
abandoned in nature, constituting a waste of natural resources and causing
environmental pollution.
2.3.1. Production coir fibers
Coir fibers are extracted from the outer shell of a coconut. There are two
types of coir fibers, brown type fibers that are extracted from matured coconuts
and white type fibers that are extracted from immature coconuts. Brown fibers are
thick, strong and have high abrasion resistance. White fibers are smoother and
finer but also weaker.
17
The total exported amounts of unfinished coir and coir products from
producing countries in 2003 and 2004 were 172,928 million ton and 194,926
million ton respectively [APCC 2006]. The Philippines are the principal coconut
producer in the world. Indonesia, India, and Sri Lanka are the followers. India is
the major coir producer in the world while Sri Lanka and Thailand maintain
second and third positions respectively. In 2007, 90% of the production came
from the Asia and Pacific region [APCC 2007]. Philippines, Indonesia, China,
Vietnam, Mexico, Venezuela, and Tanzania are the other coir-producing countries
in the world. The major importing countries of coir and coir products are United
States, European Union, Canada, Australia, Japan, the Middle East and Korea.
Nevertheless, the use of coconut husk for coir extraction is still limited to a
few developing countries while the others use coconut mainly for its kernel
products, such as copra, oil or desiccated coconut. Major coconut producing
countries like the Philippines, Indonesia or Pacific countries like Papua New
Guinea and Fiji use coconut husks and shells as an energy source for the
manufacture of copra. Because of it is the importance economic versatility (i.e.
coconut can produce food, oil, fiber and timber crop) and moreover for its,
aesthetic value. The coconut tree is popularly known as the tree of life or tree of
heaven.
Traditionally, coconut coir fiber is processed into various products such as

carpets, mats, ropes, nets, bristles, brooms, brushes, and for domestic uses with a
mattress and as coatings industry. However, only a fraction of available coir fibers
is currently used for construction materials. In recent years, the use of natural
fibers decreases due to intense competition from synthetic products. However,
there is a tendency of companies in industrialized countries to use more
environmentally friendly products and systems. This trend can help to reduce the
ecological impacts of current production methods. The effects of the chemical
industry on atmospheric degradation, global warming, declining of natural
resources, deforestation, waste production, pollution and global issues have
increased demand for environmentally friendly products.
In most areas, coir is considered as a byproduct of the production of copra

and the remaining husk at best used as fertilizer. Husk is composed of pith for 70
percent and fiber for 30 percent on a dry weight ratio [Jorg Mussig 2005]. The
ratio of long, medium and short fibers stands for the average weight ratio of
respectively 60%, 30%, and 10%. Major production areas of palm trees are found
along the coastal regions in the wet tropics of Asia in India, Sri Lanka, Indonesia,
Philippines, and Malaysia.
18
Productivity is defined as of coconut lands in the world of Nuts/ha [APCC
2008]. It appears that Brazil presents the best coconut land productivity followed
by Mexico. Indonesia has amounted to 4273 nuts/ha as shown in Figure.2.6. The
maximum total world production of coir fiber including short fiber can estimate at
5-6 million tons per year and less than 10 percent of this potential into the
commercial trade [Dam 2002].
Mexico 11,725
India 7,748
Sri Lanka 7,365
Vietnam 5,390
Thailand 4,802
Indonesia 4,273
Philippines 3,720
Malaysia 3,391
Figure.2.6. Productivity of coconut lands in the world in Nuts/ha

Source: Coconut Statistical Year Book, APCC, 2008.
It has reprocessed.
2.3.2. Extraction of coir fibers
The coconut fibers are taken from a mature coconut that is covered by fibrous
material. This part of the coconut fruit called the coconut husk, consists of hard
skin and a large number of fibers embedded in a soft material. The fibers can be
extracted only by soaking the husk in water to decompose the soft material
surrounding the fibers. This process, called retting, is widely used in developing
countries. Alternately, a mechanical process can be used to separate the fibers.
The best-quality of coir fiber is extracted from the husk of ripe-harvested

before the husk has completely dried. In general, extra carried in bulk and
commercial is as follows:
1. The extraction of coir involves the breakdown and the separation of the
coir fiber bundles from the connecting tissues or pith in between the fiber
bundles. The extraction of coir fiber is done manually by beating the retted
husks. The bristle coir or long fiber bundles have a smaller amount of
19
residual pith. Therefore, bristled fiber bundles are cleaned by combing
through a set of steel spikes. The coir fibers are sometimes, but not always,
washed with clean water and dried to give a better appearance.
2. Another way to extract fiber bundles from the machine and mattress coir
(medium and short fiber bundles) is to use the traditional drum pairs
consisting of a cone-shaped revolving screen sifter. By gravitational
action, fiber bundles are separated from the pith tissues. The coir is then
fed into a turbo cleaner, which consists of radially fixed iron rods rotating
at high speed, for further cleaning. By centrifugal action, remaining pith
tissues and other debris attached to the fiber bundles are removed by this
mechanical process. Moreover, better quality of coir is obtained.
There are four different types of coir fiber, which are produced commercially
as well as bristle fiber bundles, omat fiber bundles, mattress fiber bundles and
mixed fiber bundles. [Jorg Mussig 2010]
1. Bristle Coir: long, parallel, clean fiber bundles produced from retted coir
husks on the traditional needle drum or the deferring machine. Bristle coir
has unique features and is still competitive with other coir fiber types
produced in other countries. They are mostly used in the manufacture of
brushes, rubberized coir fibers, nettings, and high-strength twine.
2. Omat Coir: medium-length fiber bundles produced on the traditional
needle drum and the deferring machine with length ranging between 70
and 135 mm.
3. Mattress Coir: short fiber bundle fraction collected on the traditional
needle drum or the deferring machine and give length ranging between 30
and 69 mm. Those small fibers are considered as waste and are just
valorized as a plant fertilizer.
4. Mixed Coir: fiber bundles extracted from matured green husk or brown
husks, with lengths ranging between 36 and 119 mm.
Asasutjarita et al. have already studied pretreatments of coir fiber by washing

and boiling them to remove the impurities on the coir surface. [Asasutjarita,
2009]. Regarding surface topology, pretreatments can create voids and produce
fiber fibrillation, leading to a better fiber/matrix adhesion, and, therefore, better
mechanical properties of coir fiber reinforced cement composite.
2.3.3. Physical and chemical properties
Coir fiber obtained from coconut husk is a mostly under vaporized raw
materials. It is composed of cellulose nanofiber that constitutes 32–43% of its dry
20
weight [Ayrilmis, 2011]. The coir husk is another significant source of cellulose.
The coir fiber comprises mainly of cellulose, lignin, and hemicellulose.
The color of coir fibers varies from pale yellow to dark brown. It mainly
depends on the coconut variety, the maturity of the fruit, time lapsing between
husking and retting, quality of water used for retting and the duration of retting.
Coir fiber is a coarse fiber bundle. In comparison with other natural fibers, they
have high lignin content. As consequence, coir fibers are highly resistant to
microbial attacks and sea water.
The length of coir fiber bundles varies considerably within a sample. The
size of a coconut varies with the coconut variety, with the location in which it
grows and also with the environmental conditions. As for all natural fibers, it is
statistically more accurate to express the length of coir fiber bundles within a
range. There is a significant variation in length distribution with the type of
extraction technology used and fiber grade produced. Coir fiber bundles are
coarser for a natural fiber, and their diameters vary from 50 to 200 μm [Leson
2002]. Weighted average diameter at the mid-point of a coir fiber strand also
varies with coconut type.
The capacity to absorb moisture from the surroundings is a noticeable

characteristic of all natural fibers. The absorption of moisture changes the
properties of coir such as tensile strength, elastic recovery, electrical resistance,
and rigidity. Due to absorption of water, the fibers and the fiber bundles tend to
swell leading to increasing dimensions. As a consequence size, shape, stiffness
and permeability of products such as yarn or ropes can also vary. When a dry fiber
or fiber bundles exposed to the atmosphere, they will take up moisture from the
surroundings and reach equilibrium. Similarly, when they are exposed to a dry
climate, moisture is lost on the surroundings to establish a new equilibrium. The
amount of water in coir fiber could be expressed regarding humidity or moisture
regained. Nawaratne et al. found that the moisture content of fresh-water-retted
fiber samples was 10.20% with moisture regain of 11.31% when they are sea-
water-retted. The coir was 7.92% with moisture regain of 8.60% [Nawaratne
2002]. Thus, retting methods have some effects on the moisture absorption of coir
fiber bundles. Physical properties of coir fiber are given in Table 2.5.
As with other vegetable fibers, the main chemical components of coconut

fiber bundles are cellulose, hemicellulose, pectin, and lignin. In most plant fibers,
more than 70% consists of cellulose. In contrast, coir has high lignin content and
a lower amount of cellulose [Dam, 2002]. Cellulose is a metabolically inactive
structural carbohydrate, a polysaccharide consisting of a linear chain.
Hemicellulose is another polysaccharide with a random, amorphous structure,
21
contained many different sugar monomers and associated with cellulose. The
combination of cellulose and hemicellulose is known as holo-cellulose. Lignin is a
polymer of phenylpropanoid units. Lignins are formed from three other phenyl
propane‘s, alcohols (monolingual monomers) called coumarin alcohol, coniferyl
alcohol, and sinapic alcohol.
However, these compounds can vary with the maturity of the fruit, as well
as with the coconut variety. Lignin in the cell walls gives rigidity and color. It also
reduces the permeation of water through the cell walls. Lignin also plays a
significant role in the transport of water, nutrients and metabolites in the vascular
system of plants. Furthermore, lignin in plant cells helps to maintain rigidity of
the cell wall and gives resistance towards compression and bending, as well as
protection against attack by microorganisms.
Table 2.5 The physical properties of coir fibers.

Reference Diameter Length Density Moisture Water
Content Absorption
Saturation *
Ramakrishna& 0.40 - 0.10 60 -250 - - -
Sundararaja mm mm
2005b
Agopyan et al. 210 µm - - - 93.8 –161 %
2005 c
Paramasivam et 0.3 mm - - - -
al. 1984
Ramakrishna& - - - - 180 %
Sundararaja
2005a
LI et al. 2007 270 ± 73 50 ± 10 - 10% m 24 % l
µm mm
Toledo Filho at 0.11 – - 0.67 –10 - 85.0 –135 %

al. 2005 0.53 mm g/cm3
Munawar at al. 121.3 ± - 0.87 - -
2007 4.9 µm g/cm3
Rao and Rao et - - 1150 11.36% -
al. 2007 Kg/m3
Fernandez 2002 - - 1.2 g/cm3 - -
Reis 2006 0.1 - 0.4 - - - -

mm
22
Aggarwal 1992 0.1 - 0.4 50 -250 145-280 - 130 - 180 %
mm mm Kg/m3
Satyanarayana 100 - 450 - 1150 - -
et al. 1990 µm Kg/m3
Source: [Majid Ali 2012]. Has been reprocessed
[Satyanarayana 1982] found that cellulose content varies from 33 to 43%,

lignin from 41 to 46%, hemicellulose from 0.15 to 0.25% and pectins from 2 to
4%. The property of resistance of coir to degradation, when attributed to its high
content of lignin (30% or more) compared with other plant fibers such as cotton
and jute [Rao 2002].
Coconut coir fiber is on average composed of 46% of lignin (weight
basis); it is one of the natural fibers containing the higher lignin content [Khedari
2004]. Lignin can be extracted selectively and progressively by treating the fibers
with an alkaline aqueous solution or an organic solvent [Le Digable 2006]. It is
thus a medium to conduct a systematic study on the effect of lignin on bio-
composites properties.
2.3.4. Mechanical properties
Ramakrishna and Sandararajan investigated the effect of variation in

chemical composition of tensile strength of four natural fibers (coir, sisal, jute and
cannabinus fibers) when subjected to alternate wetting and drying, and continuous
immersion for 60 days in three mediums (water, saturated lime and sodium
hydroxide) [Ramakrishna and Sandararajan 2005b]. Chemical compositions of all
fibers are affected by the immersion conditions.
Table 2.6 Mechanical properties of coir fibers.

Reference Tensile strength Elongation Young‘s
Modulus
Ramakrishna& 15 - 327 N/mm2 0.75% -
Sundararaja 2005b
Agopyan et al. 2005 c 107 MPa 37.7 % 2.8 GPa
Paramasivam et al. 69.3 N/mm2 - 2.0 x 103

1984 N/mm2
Ramakrishna& 50.89 MPa 17.6 mm -

Sundararaja 2005a
LI et al. 2007 142 ± 36 MPa 24 ± 10 % 2.0 ± 0.3 GPa
23
Toledo Filho at al. 108.26 –251.90 MPa 13.70 –41 % 2.50-4.50 GPa
2005
Munawar at al. 2007 137 ± 11 MPa - 3.7 ±0.6 GPa
Rao and Rao et al. 500 MPa - -

2007
Fernandez 2002 175 MPa 30% 4.0 - 6 GPa
Reis 2006 174 MPa 10-25 % 16 - 26 GPa
Aggarwal 1992 100-130 N/mm2 10-26 % 19 -26 N/mm2
Satyanarayana et al. 106 - 175 MPa 17 - 47 % 4.0 -6 GPa
1990
Source: [Majid Ali 2012]. Has been reprocessed

Continuous immersion is found to be critical, and fibers lost their strength.
However, coir fibers were reported to present the best tensile strength retaining
the ability for all tested immersion conditions.
Munawar et al. characterized the morphological, physical and mechanical

properties of the non-wood plant fiber bundles (ramie, pineapple, sansevieria,
kenaf, abaca, sisal and coconut fiber) [Munawar 2007]. The larger the diameter of
the fiber bundles, the lesser will be the density, tensile strength, and the Young‘s
modulus.
2.3.5. Thermal properties
The Energy conversion of coir is little [Rowell 2002]. With its high
percentage of lignin, coir fiber possesses natural resistance to soiling and
dampness. In hot climates, it gives cool comfort and in cold weather it retains
warmth. It also has good stretching and shrinking ability. Because of these
favorable properties, it is widely used for floor covering all over the world. Coir
fiber can be dyed and printed easily to get the desired colors and designs with
lasting finish. It can also absorb sound waves, and because of its superior acoustic
qualities it frequently used for wall paneling and floor covering in auditoria and
concert
The presence of lignin–cellulose compound in the raw coir fiber plays a

significant role in its structural and thermal properties of the fiber. [Abraham
2013] The extracted lignin is also a suitable source for renewable energy
production.
2.3.6. Microstructure
24
The SEM micrographs of the coir fiber at different processing stages are
shown in Figure.2.7. The SEM micrograph of the natural raw coir fiber is shown
in Figure.2.7 (A). The fiber surface appears to be smooth due to the presence of
waxes and oil. However, the presence of pores could be observed on the surface.
Though coir fiber has high lignin content (49.2%), the moisture absorption
capability is comparable (9.2%) with the other fibers (Table.2.6). Figure.2.7 (B) is
the SEM micrograph of an alkali treated fiber. The arrangement of cellulose fibers
within the matrix of lignin is clearly seen in this picture. The removal of
cementing materials, primarily lignin, from the surface of the natural fiber, occurs
during this step.
Table 2.7 The chemical properties of coir fibers.
Cellulose Lignin Hemicellulose Moisture

Content
(%) (%) (%) (%)
Raw coir fiber 39.3 (±4) 49.2 (±5) 2 (±0.5) 9.8 (±1)
Alkali treated fiber 50.5 (±3) 38.8 (±4) <1 10.3(±1
Source: [Abraham, 2012]. Has been reprocessed
Figure.2.7. SEM pictures: (A) raw coir fiber, (B) alkali treated coir fiber
Source: [Abraham 2012].
25
2.4. Natural fiber reinforced cementitious composites.
Applications of natural fibers in composites used for building purpose

have been performed for centuries. Examples, in the Egypt of Pharaohs, Israel or
China show the reinforcement of clay bricks by natural straw. Fiber reinforced
cement-based composites can use for many applications in civil engineering. For
example, fiber reinforced cementitious tiles [Agopyan 2005], corrugated roofing
sheets [Paramasivam 1984], simple slab panels [Ramakrishna, 2005], wallboard
[Li 2007] [Asasutjarita 2007], and mortar [Toledo Filho 2005]. There have
reported in the recent literature. Currently, the construction is the largest are of
application of fiber composites (in volume).
Natural fibers have a low environmental impact comparing to synthetic or

steel ones. As a result, they are suitable to design eco-friendly building materials.
Fiber reinforced concrete can absorb seismic waves like a massive stone. Concrete
made with flexible fiber reinforcements can withstand earthquakes [Shelly 2006].
Since ancient time, fibers are added to brittle materials to give them more
tensile strength and more ductile properties. Since 1910, steel wire is attached to
cement-based materials. Later studies using glass fibers in cement took place in
the50‘s. In the 60‘s, the synthetic fiber was also examined as concrete
reinforcement. Since 1970, the study of natural fibers, to replace relatively
expensive synthetic fibers, began. Gradually since 1980, research has been
conducted on the characteristics of coconut fiber from tropical countries such as
India, Brazil, Malaysia, Thailand, Vietnam, Sri Lanka, Bangladesh, and Tanzania.
The applications of materials made of natural and local resources have

increased worldwide. Their significant variation in properties and characteristics
is the greatest challenge in working with natural fiber reinforced composites.
Some variables, including the fiber type, environmental conditions where the
plant fibers sourced, processing methods, and any modification of the fiber
influence composite properties. Products processed with Portland cement blended
with natural fibers such as coconut, sisal, bagasse, bamboo, hemp, wood and
vegetable fibers. It has shown to be suitable to add to construction materials [Aziz
1981], [ Paramasivan 1984]. Although the results are encouraging, there are some
drawbacks especially some durability issues. It seems that the interface between
fiber and cement paste is affected by the fiber swelling in the presence of
moisture. For that reason, some researchers are now investigating remedial
measures for improving durability. Accordingly, natural fiber-reinforced cement
composites are most suitable. It is for earthquake resistant construction,
foundation floor for machinery in factories, fabrication of lightweight cement-
based roofing and ceiling boards, wall plaster, and building materials for low-cost
26
housing [Aziz 1981]. The use of natural fibers in the construction industry will
help to achieve sustainable patterns of consumption of building materials.
Natural fibers used as reinforcement in concrete is a cost-effective

replacement for expensive, high energy consumed and non-renewable fibers
[Pacheco 2011]. Recently, the use of natural fibers to replace carbon/glass fibers
as reinforcement in fiber-reinforced polymer composites has gained popularity
due to increasing environmental concern. Natural fibers are low-cost fibers with
low density. They are Biodegradable, non-abrasive, renewable, recyclable,
required reduced energy consumption and present less health risk. Also, they are
readily available, and their specific mechanical properties are comparable to those
of glass fibers used as reinforcement [Malkapuram 2008]. Therefore, natural
fibers represent a highly ―sustainable‖ material. The use of natural fibers in fiber
reinforced concrete composites as building materials will promote the
―sustainable‖ development in the construction industry
The natural fibers are used for a long time in many developing countries in
cement composites because of their availability and low cost [Ghavami 1999]
[Savastano 2000]. Also, for low-cost building construction in developing
countries, natural fiber-reinforced cement composites are found attractive
[Ramakrishna 2005]. Un-reinforced cement concrete has low tensile strength and
low strain capacity at fracture. Then researchers began looking for other
alternatives for concrete reinforcement. Along with an increase in the
environmental awareness in the world, researchers have focused their work on the
valorization of bio-based high-performance materials such as natural fibers.
Natural fibers are locally available in many countries. So their uses as a
construction material for increasing properties of composites at a very little cost
(almost nothing when compared to the total cost of the composites) are very
promising. Moreover, their use can lead to having sustainable development
[Ramakrishna 2005].
The researchers have used plant fibers as an alternative to steel fibers in

the manufacture of fiber composites such as cement paste, mortar, and concrete.
For example, natural fibers blended cements include coir, sisal, jute, hemp bast,
pineapple leaves, kenaf bast, leaf abaca, bamboo, banana, flax, cotton and
sugarcane [Ramakrishna 2005] [ Agopyan 2005] [Li et al., 2007] [Asasutjarita
2007] [Toledo Filho 2005] [ Munawar 2007] [ Rao 2007] [Li 2006] [Fernandez
2002] [Reis 2006] [Corradini 2006].
A problem of workability arises when a high percentage of fibers is

incorporated into a fresh mix, as in the case of steel fibers [Martinie 2010].
Volume fraction and fiber content are two terminologies used for expressing the
quantities of fibers in a given composites [Ramakrishna 2005] [Agopyan 2005]
27
[Paramasivam 1984] [Li 2007] [Asasutjarita 2007] [Toledo Filho 2005] [Li 2006]
[Fernandez 2002] [Reis 2006] [Aggarwal 1992] [Corradini 2006] [Toledo Filho
1999]. The various researcher has already studied uses of coconut coir as
reinforcement in cement. Among them, a study on the feasibility of cement board
[Asasutjarita 2009] or the durability of coir cement composites [Toledo Filho
2000] is reported.
Natural fibers are a valuable renewable resource materials; the substitution

of steel fibers by coconut vegetal fibers presents many advantages because the
coir is an abundant, versatile, renewable, cheap, and biodegradable lignocellulosic
material.
2.4.1. Rheological behavior
In the building industry, fresh concrete flowability is required to ensure a

smooth casting and to keep the mix homogeneously. This property is defined as
workability. The workability of concrete depends on their rheological properties.
Concrete or more cement-based materials are mainly considered to behave as
Bingham materials. The Bingham behavior is modeled using two parameters: the
yield stress and the plastic viscosity.
Fibers have a very positive influence on the mechanical properties of

cementations materials in the hardened state. This impact depends primarily on
the fibers (shape, constitutive material, volume fraction) but also on the casting
process. Indeed, contrary to traditional aggregates, flow, in the case of fiber-
reinforced materials. It can induce a preferred orientation of the fibers, which
actively modify both fresh and hardened material properties as presented by
[Martinie 2010].
The yield stress, plastic viscosity, and thixotropy are important rheological
parameters to analyzes fresh concrete. Newtonian liquids, such as water and oil,
show a linear relationship between shear stress (τ) and shear rate ( ) as shown
in Figure 2.8 as:
τ=η …………... (2.1)
Where: η is the viscosity. There is considerable evidence that the cement-based

materials behave as a Bingham material. The Bingham model can be modeled as
follow:
………………….(2.2)
28
If 𝜏 ………………….(2.3)
Where: τ is shear stress (Pa), Is the shear rate (1/s), τo is the yield stress (Pa),
and μ is a plastic viscosity (Pa-s) respectively. If the shear stress is lower than the
yield stress, the material behaves as an elastic solid but when the yield stress was
exceeded, the material start to flow. Yield stress is the critical shear stress
required to initiate flow deformation and is directly linked to entering particular
forces. As shown in Figure 2.8, the plastic viscosity is the slope angle of the shear
stress vs. shear rate relationship.
Figure 2.8. Newtonian and Bingham flow, models
Thixotropy is also an important rheological term to describe fresh

concrete. Thixotropy is a decrease of apparent viscosity under shear stress,
followed by a gradual recovery when the pressure removed. The effect is time-
dependent [Barnes 1997]. Thus, after the concrete casting into the form, a
structural build-up occurs, and both yield stress and viscosity increase. To some
extent the concrete, supports its weight that results in little pressure on formwork
and a high casting rate [Koehler 2005a]. The thixotropic property reduces the risk
of segregation after placing.
Figure 2.9 taken from Newman and Choo shows the effects of different
materials on the rheological properties for concretes, in general [Newman 2003].
Incorporation of super plasticizers dramatically decreases the yield stress but has
only little effect on viscosity. Compared with superplasticizers, water decreases
both the yield stress and the viscosity (however, it also drastically decreases
concrete strength).. The side effect of the change in water content in concrete is
that it may induce bleeding or segregation. Viscosity modifying admixtures can be
added to prevent any segregation risk by increasing the viscosity without affecting
the yield stress. The paste is another important factor on the Bingham parameters.
29
The addition of paste will result in a decrease in yield stress and increase in
viscosity. Using supplementary cementitious material such as fly ash leads to a
decrease in the yield stress of concrete.
It is worth to note that the rheology of cement-based materials influences

the orientation of the fibers during casting or extrusion.
Figure 2.9. General effects of concrete constituents on the Bingham

parameter
Source: [Newman 2003]
2.4.2. Physical properties
Sugar components of fiber such as hemicellulose and lignin may interfere

with cement hydration. Savastano mentioned that acid compounds released from
natural fibers increase the setting time of the cement matrix [Savastano 2003a].
According to Sedan, fiber inclusion can increase the delay of setting by
45 min. It relies on the fact that fibers pectin can fix calcium preventing the
formation of CSH structures [Sedan 2007].
2.4.3. Mechanical properties
Fiber characteristics such as tensile strength, elastic modulus, diameter or

length affect the mechanical properties of fiber-reinforced composites. Fibers
dispersion and orientation within the matrix play also an important role. The bond
strength of the fiber-matrix interface is essential to reach high mechanical
properties. Also, factors like processing conditions/techniques have a significant
influence on the mechanical properties of the fiber reinforced composites. The
30
most important characteristic of the composites is their strength. Their high
mechanical strength combines with they're a relatively low weight for optimized
use in engineered structures such as ships, cars or buildings. Composites tensile
strength can be four to six times greater than that of steel or aluminum [Biswas
2002]. Structures made of composites are 30-40% lighter than similar ones made
of aluminum.
Environmental interactions influence the strength of composites. A recent

study shows that the tensile strength of composite resins presents lower values
after storage and test in water as compared to the dry condition due to its water
absorption [Tani 2002]. Tensile strength expressed as the breaking load per unit
cross-sectional area of the test specimen is an important physical property of
fibers. 34% can increase the fiber tensile strength, fiber toughness and fiber–
concrete bond strength, 55%, and 184%, respectively when fibers are boiled and
washed [Ali 2013].
The flexural strength can be slightly increased by using only coconut fiber.
Natural fibers such as coconut are reported to improve the compressive and tensile
strength of cement based composites [Asasutjarit 2007]. Likewise, fracture
toughness and fracture energy of polymer concrete can be increased by using
chopped coconut fiber and sugarcane bagasse fiber [Reis 2006].
The use of natural fibers in the cement matrix leads to lightweight

materials with excellent tensile behavior. Previous researchers on fiber reinforced
concrete have shown that short natural fibers can modify tensile and flexural
strength, toughness, impact resistance and fracture energy of cementitious
materials [Pacheco 2011].
Pacheco-Torgal and Jalali reviewed the mechanical impact of several

vegetable fibers (i.e. sisal, hemp, coir, banana and sugar cane bagasse) as
reinforcement in cementitious building materials. Among those natural fibers, coir
fiber presents some advantages to being used as reinforcement. Its highest
toughness among natural fibers, it's extremely low cost, as well as its availability
[Baruah 2007] makes coir fiber very interesting. Li et al. stated that flexural
toughness and flexural toughness index of cementitious composites with coir fiber
are increased by more than ten times due to coir fiber bridging effect [Li 2004].
Reis also reported that coir fiber increases concrete composite fracture
toughness. Moreover, the use of coir fibers shows even better flexural properties
than synthetic fibers (glass and carbon) [Reis 2006]. Therefore, the inclusion of
coir fiber might be useful to increase the flexural performance of concrete
composites, particularly in changing the brittle failure pattern of the concrete core.
31
Meanwhile, according to Filhoa et al. [Filho 2000], cementitious
composites made with coconut fiber present a significant decrease in toughness
after six months out of aging or submitted to cycles of wetting and drying.
Majid Ali et al, show that fibers have the maximum bond strength with
concrete when (i) embedment length is 30 mm, (ii) fibers are thick, (iii) fibres are
treated with boiling water, and (iv) concrete are mix designed with ratio of one
mass of cement; 3 masses of sand; 3 masses of gravel [Majid Ali 2013].
Single fiber pull-out tests have been carried out to determine load–slippage
curves with the help of an Instron tensile machine fitted with a load cell. Bond
strength and energy required for fiber pullout are computed from experimental
data [Majid Ali 2013].
The use of natural fibers in concrete is not only useful to improve the
mechanical properties of concrete, but also promote the sustainable development
of green concrete and thus conserve natural resources [Awwad 2012].
2.4.4. Thermal properties
Measurements of the thermal properties have been performed by [Khedari

2002] and [Asautjarit 2007] on cement-based composites containing coconut coir
fibers. Coir fiber is an interesting product because it has low thermal conductivity
and bulk density. The development of composite materials for buildings using
natural fibers such as coconut coir can then help to improve the energetical
efficiency of the building.
Asasutjarita et al. determined the physical, mechanical and thermal

properties of coir fiber-based light weight cement boards after 28 days of curing
[Asasutjarita 2007]. The parameters studied were fiber length, coir pre-treatment,
and mixture ratio. After being boiled and washed, 6 cm long fibers gave better
results. On the other hand, optimum mixture ratio by weight of cement; fiber;
water was 2:1:2. Also, the tested boards had a lower thermal conductivity than
that of commercial flake board composites.
Assessment of thermal characteristics of coconut fiber and its use to

modulate the temperature of concrete slabs in the construction industry are
presented by Rodriguez [Rodriguez 2011]. This study indicates that fiber located
on the outer surface of the concrete allows the room temperature to be in the range
of comfort.
32
2.4.5. The fiber–matrix interface
There are several factors related to natural fibers that influence the
performance of the composites such as an interfacial bond, fiber orientation,
tensile strength and, chemical fiber properties. The reinforcements are the solid
part of the composites, which reinforced into the matrix. They determine the
strength and stiffness of the composites. In terms of reinforcing effects, lignin
removal has no significant impact on composite mechanical properties but slightly
reduces the water absorption of samples.
The mechanical efficiency of the fiber-reinforced cement composites

depends on the fiber–matrix interface and the ability to transfer stress from the
matrix to the fiber as reported by many researchers.
The fiber composition depends on the plant from which it has been
extracted, and the agricultural conditions. It is mainly composed three
compounds. There are cellulose, hemicellulose, and lignin. Moreover, the local
repartition of the compounds is not homogeneous. In general, lignin mainly
located at the surface of the fiber while the backbone is mainly composed of
cellulose. Adhesion between matrix and fiber is an important parameter affecting
the mechanical properties. A composite with excellent adhesion ensures a good
stress transfer from the matrix to the fiber [Riande 2000].
The realization of the mechanical performance of the reinforcement is

critically dependent on the effective load transfer by shear over the critical half-
length at each fiber end. These are a function of the chemical -physical bonds
between the fiber and the matrix. The main approaches to enhance the interaction
between the fiber and the matrix are surface modification of the fiber (grafting or
other chemical/physical treatments), application of coupling agents to the fiber
surface and/or the use of compatibilizers in the matrix. George et al. have
critically reviewed the physical and chemical treatments that may improve the
fiber–matrix adhesion [George 2001].
Single fiber pullout tests are performed to determine the bond strength and
the energy required for fiber pullout. The experiments on fiber tensile and fiber–
concrete bond strength reveal that, thick (0.30–0.35 mm diameter) boiled fibers
have higher tensile strength compared to the thin (0.15–0.20 mm diameter),
medium (0.20–0.30 mm diameter), soaked and chemically treated fibers. The
bond strength increases with embedment length and has the highest value at 30
mm embedment. Furthermore, Ali present that pullout energy increases with a rise
in embedment length. Thin fibers in concrete with a 1:3:3 mix design ratio. The
medium fibers in concrete with a 1:2:2 mix design ratio break because the pullout
33
load is higher than the fiber tensile strength. The thick fibers have the bond
strength and tensile strength of 37 and 82 MPa, respectively [Majid Ali 2013].
2.5. Extrusion of cementitious composites
In recent years, the processing and production technologies for cement-

based composites have also advanced. To date, injection molding, extrusion,
compression molding, sheet molding and self-consolidating paste are the primary
manufacturing processes for natural fiber-reinforced cement-based precast
composites. Hence, new downstream and auxiliary equipment has been designed.
Cement-based materials can be classified as cement paste (cement +

water), mortar (cement paste + sand) and concrete (mortar + gravel). They are
used as materials for the building industry. Cement-based materials were
commonly cast in place. However, new engineering composites are now precast
in dedicated factories. Then the use of extrusion is intended to optimize the
manufacturing process of precast elements.
Extrusion of cement-based materials can be a high productivity forming

process. The extrusion process can form hardened cement composite with higher
mechanical properties compared with traditional casting process [Mu 1999]
[Peled 1999].
Hence, it is expected to improve the mechanical properties of the

processed materials. However, it has not yet become a common way to form
cement-based material in an industrial setting. The mechanism that regulates the
flow of mortar or cement paste extrusion is an important point for the
development of viable industrial extrusion process for cement-based materials.
The material becomes softer and plug flow zone in which the material becomes
more difficult on part of the liquid phase can flow through the die and creating a
shared zone. Such phenomenon has to be avoided to ensure extrusion success
[Perrot 2009]. Then, extruders must be optimized to provide homogeneous
extrudates at high speeds to ensure the industrial processing of the material.
This process is developed and used since a long time for the perfect and
homogeneous plastic and viscoplastic materials. In this case, the stress distribution
and the material flow have been well described. It is not the case of more complex
materials such as cement-based pastes. For these saturated and concentrated
suspensions which present high solid volume content, extrusion should be an
interesting way to decrease their porosity and improve their mechanical strengths,
which are the main characteristics of building materials. However, it has been
34
observed that very concentrated suspensions are likely to undergo liquid filtration
during their extrusion [Perrot 2007] [Perrot 2009] [Khelifi 2013].
According to Toutou et al., a granular paste must have an internal yield

stress around 20 kPa to be suitable for extrusion [Toutou 2006]. This critical value
corresponds to a paste firm enough to keep its shape at the extruder outlet and
sufficiently ―soft‖ to limit extrusion force due to plastic deformation and internal
friction. Several recent studies suggest that cement-based materials are likely to
undergo drainage during extrusion. Authors have proposed criterions based on
filtration velocity linked to paste permeability. Stress distribution, internal
friction, and wall friction remain constant if extrusion process is largely faster
than the filtration. In this case, the material remains homogeneous, its behavior
remains viscoplastic, and the process corresponds to a proper extrusion. On the
contrary, if filtration is allowed by a low speed of extrusion, solid volume fraction
increases and particles may percolate.
If the percolation threshold was reached, the material behavior becomes

frictional. As a result, shear and friction stresses largely increase [Lecompte
2012]. In this case, normal forces due to shearing appear and induce an internal
friction increase [Khelifi 2013]. It was also shown that drainage appears for low
extrusion velocity when viscous effects may be neglected. A growing
consolidated area located at the ram may appear. In this case, extrudates contain
more liquid than the initial mixture. This material heterogeneity leads to an
increase of the extrusion load and unsuitable extrudate quality. In the worst case,
it can lead to a process blockage (Figure 2.10). Filtration occurs; the material
becomes heterogeneous in the extruder
35
Figure 2.10. Evolution of the extrusion according to the ram advance for
different speeds of extrusion effort.
Source: [Perrot 2009].
The surface quality of the extrudate is also an important characteristic of

the extrudates. The periodic appearance of defects on the surface of the material
studied is shown in Figure 2.11. The period of occurrence of defects seems to
depend on the extrusion speed and appears to disappear for sufficiently high
speeds [Lanos 2004]. The periodic appearance of the defect seems too related to
the friction conditions at the wall. The authors conclude that the phenomenon of
speed dependency is due to the phenomenon of drainage and reorganization of
pore pressures during extrusion at slow speed. It is confirmed by the study of the
extrusion type flow [Perrot 2009].
Figure.2.11. The appearance of the surface defects according to the extrusion

speed.
Source: [Lanos 2004] has reprocessed
36
During the process of shaping material, the conditions of contact between
the surfaces of the forming tools and the material may change significantly. The
knowledge of the type of tribological behavior at interfaces is, therefore,
necessary to understand and optimize the flow conditions during processing.
Furthermore, the tribological behavior near the die may have a significant
influence on the appearance of the extrudate defects in the particular case of
materials with a very marked plastic behavior.
2.5.1. Extrudability of cementitious materials.
Pates must meet some criteria to be extrudate. During extrusion, the

problem of drainage and consolidation of paste flow has to be taken into account
in order to optimize extrusion conditions. Heterogeneities can occur and affect the
quality of the extrudate [Perrot 2006]. On the other hand, Toutou develops a
method for optimizing the composition of mortars and cement pastes from the use
of simple compression test (also called squeeze flow). As an identifier of the
rheological behavior and the field of extrudability. A criterion of the surface
appearance and dimensional stability of the extrudate fresh is then defined to
describe an entire extrudability field (Figure 2.12) [Toutou 2005]. In order to
sustain gravity and handling, the paste has to present a minimum yield stress
value. The author sets this parameter to 20 kPa.
Other criteria related to the homogeneity of the material during extrusion

established; they seek to avoid surface defects and heterogeneity of the extrudate
induced by the phenomenon of drainage [Perrot 2009]. In this study, the author
performs an analysis based on the mechanisms of filtration of the fluid through
the granular skeleton, leading to the definition of a criterion based on the
extrusion rate. It to avoid the appearance of heterogeneities. Concepts of soil
mechanics (consolidation theory, Darcy's law) are related to the concept of
rheology and used to describe the permeability of the granular skeleton and the
kinetics of drainage. A dimensionless number, defined as the ratio of extrusion
time to the time needed to double the yield stress of the paste during the flow as
the reference criterion for filtration effects.
37
Figure.2.12. Border field of extrusion of plastic material - no effect - speed
according
Source: [Toutou 2002]
2.5.2. Extrudability of fibers cementitious materials.
Extrusion technology has been used for the production of cement boards
with unbleached kraft pulps. Extrusion was found to be a suitable process for
cement boards with up to 8% pulp by weight. Higher pulp content increases the
toughness of the material but does not enhance the flexural strength due to higher
water content required for extrudability. Hardwood pulps, cheaper and more
available than the softwood ones, were found to be more suitable for extrusion
production in terms of extrudability [Shao 2002]. Extrusion allows incorporating
both hydrophilic and hydrophobic fibers into fiberboard production. It found that
sand content had a significant effect on toughness. The more the sand added, the
less the toughness is. In this study, fiber dispersion seems not to be critical.
Fiberboard made by non-dispersive mixing exhibited acceptable performance.
Accordingly, the mixing time and energy in extrusion production could, therefore,
be reduced.
Shao presents a comparative study of cementitious sheets extruded fibers

of polyethylene terephthalate (PET), glass, polyolefin (PO) and PVA. The flexural
strength of the plates with glass fiber presents the highest deformation at failure.
SEM analysis shows that the plates of PVA exhibit good fiber - matrix adhesion
and thus a larger energy are consumed for the tear in the fiber matrix [Shao et al.
2001].
38
The use of hybrid glass/carbon fiber reinforcement has shown efficiency.
The fiber is a very convenient solution for strengthening reinforced concrete
structures [Qian 2003]. The hybrid compound, a mixture of two or more types of
fibers is a very advantageous solution for strengthening cementitious materials.
Also, a hybrid combination of appropriate fibers can potentially improve global
concrete properties. This concept has also been tested on extruded cementitious
materials. While glass fiber reinforcement primarily improves the tensile strength,
reinforcing PVA fibers improve the ductility. The use of a hybrid combination of
glass and PVA fiber induces improvements brought by the large deformability of
PVA fibers and the glass strength. However, the tensile strength is lower than that
of glass fiber reinforced composites [Mu 2000], [Li 2001].
The analysis of the state of the art on cementitious extruded material

shows that extrudates are denser and has better bonding between fibers and
matrix. [Akkaya 2000c], [Akkaya 2001], [Shao 2001], [Qian 2003]. Akkaya et al.
compared the material properties of extruded and molded cement containing PVA
fiber reinforcement of different lengths (2, 4 and 6 mm for extruded materials, 2
and 4 mm for cast materials). The tensile strength, the flexural strength of the
extruded material decreases with the length of the fiber while it increased with the
fiber length when the material was cast. This contradiction is associated with
differences in failure mechanisms and the change in fiber dispersion and
orientation [Akkaya 2000b]. Peled and Shah studied the effect of fiber length (3%
by volume of PVA and acrylic fibers 2 and 6 mm). Moreover, the substitution of
cement by fly ash on the mechanical characteristics of extrudates confirm the
results obtained by Akkaya [Akkaya 2000b] and show using microscopic
observations that extrusion improves fiber-matrix bond [Peled 2003].
2.6. Environmental impact
Many researchers have conducted studies to assess if plants can provide

interesting raw materials for composites to reduce their environmental impacts.
The use of composites has reduced the impacts on the environment as it has
reduced the use of various toxic compounds. Houses may be built in earthquake
zones using lightweight composites and may help in reducing the impact on
human life when disaster strikes. Lightweight composite structures have increased
fuel efficiency in cars, buses, ships.
During construction design, one of the important things to consider is

insulation nowadays. It helps reducing energy losses and to retain the internal
temperature. The construction industry is a major consumer of natural resources
and energy, have a strong impact on the environment. Cement production process
39
produces CO2 emissions that give a high environmental impact. From the total
greenhouse gasses emitted by this sector, 50% are directly resulting from
transportation, manufacturing and use of materials in the construction phase
[Habert 2009]. It is necessary to evaluate the environmental impact of the product.
It can be mass using Life Cycle Assessment (LCA) method.
2.6.1. Life cycle assessment methodology
Today the world is working towards a sustainable environment. People

tend to be aware of their environment and want to know more. Many tools are
designed to study the impacts on the environment and to help producers, decision-
makers, and consumers to decide what to choose as an environmentally friendly
product and bring it into use. Similarly, Life Cycle Assessment (LCA) is a tool
use to assess the present and future impacts of any construction.
LCA is now a part of the International Organization for Standardization

ISO 14040-14044 which issued in 2006. The term 'lifecycle' refers to the notion
that holistic assessment the raw material production; Manufacturer; distribution;
use and disposal (including all intervening transportation steps). These inputs and
outputs are then converted into their effects on the environment to assess, their
environmental impacts [ISO 14040, 2006].
LCA is used now for the past 10-15 years. It has helped to provide
grounds for decision makers, political bodies and consumers to make the right
choice, which is more sustainable and safe for the environment, in the long run.
Boundaries for the study were set. The functional unit has to be defined.
For e.g. functional unit can be the impact per liter of packaged beverage. In this
phase, the impact categories and methods that will be used to study the impacts
are also discussed.
In the inventory analysis phase, it is defined where the data was collected.
The impact assessment phase includes three steps: classification of parameters
according to the impact categories they contribute to, characterization of the
potential contribution to each impact studied, and the last step is weighting. The
total impact over the lifecycle is usually an optional step. It can also be known as
the combination of the above two mentioned steps of classification and
characterization.
Interpretation is the last phase where all the results of the impact
assessment were discussed, keeping in mind the functional unit. It is the final step
in an LCA where we can analyze all data and come to a conclusion. It should be
40
used as a tool to find the best choice when considering different products
(comparative LCA). In the present work, LCA is used to study environmental
impacts of fiber reinforced composites for a given application (functional unit).
The construction and operation of a building cause the consumption of a

large amount of energy; they also induce a high demand for physical resources
and significant impact on the environment. The building also significantly
influences the energy consumption of future generations and the deconstruction,
recycling or disposal of the buildings will take place about 80– 100 years after the
construction. Thus, the construction sector can significantly contribute to a more
sustainable development [Zimmermann 2005]. Heavy materials and long
transportation distance will affect the outcome of transportation on Environmental
life cycle assessment (LCA). Another issue is cement production; authors have
assessed the environmental impacts associated with three alternative technologies
for the cement manufacturing process [Huntzinger 2009].
Environmental LCA is a valuable tool to understand the environmental

hazards of products. It is also used to optimize the manufacturing process to
reduce adverse environmental impacts. However, there are limitations to the
study, and it should note that data aggregation problems associated with
secondary information sources might cause variation in impact values for
replication studies. However, the results of LCA show that blended fibers cement
may provide considerable environmental savings.
2.6.2. CO2 emissions
Over the year‘s emissions from industries, car, fuel combustion,

deforestation has led to the phenomena called as the global warming. It is due to
the greenhouse effect of gasses as carbon dioxide, NOX, SOX, and methane cause
the heat to be trapped within the earth atmosphere and stop it from moving into
space. It has led to increased temperature of the land and has resulted in climate
change.
In conclusion, the available data indicate that natural fibers have a

tremendous potential as a mean not only to save nonrenewable resources but also
to control greenhouse gas emissions [Zini 2011]. The five following sectors are
the most significant contributors to CO2 emissions:
1. Fossil fuel combustion (including international transport ‗bunkers‘,
marine and aviation),
2. Fugitive is emissions from fuels,
3. Cement production and other carbonate use,
4. Feedstock and
41
5. Other non-energy uses of fossil fuels.
Global CO2 emissions have declined by 1% in 2009 and have known an
unprecedented increase of 5% in 2010 followed by a novel increase of 3% in
2011. C02 emissions have reached an all-time high of 34 billion tons, as shown in
Figure 2.14 [Olivier 2012].
Figure.2.13. Global CO2 emissions per region from fossil fuel use and cement
production.
Source: [Olivier 2012]
Globally, cement production is an indicator of national construction

activity. Cement was mainly used in building and road construction. The
carbonate oxidation in the cement clinker production process generated CO2
emissions. This principal constituent of cement is the largest non-combustion
sources of CO2 from industrial manufacturing contributed about 4% to total
global emissions [Lucinda 2012].
In total, cement production accounts for roughly 8% of global CO2

emissions [Olivier 2012]. It is especially severe in the current context of climate
change caused by carbon dioxide emissions worldwide, leading to a rise in the sea
level [Pacheco 2011].
42
The biggest emitters are in 2011: China 29%, United States 16%,
European Union (EU27) 11%, India 6%, the Russian Federation 5% and Japan
4% [Olivier 2012]. The CO2 emissions from fossil fuel used and cement
production shown in Figure 2.15.
Figure.2.14. CO2 emissions per country from fossil fuel utilization and cement
production
Source: [Olivier 2012]
43
2.7. Conclusions of chapter
Natural fiber is a renewable, sustainable material, with low environmental

impact. However, there are still problems that need attention. They were used as
reinforcement material in composites, but fiber properties are much dispersed and
water sensitive. Fibers have an irregular cross section with a central void (lumen)
which makes the determination of their mechanical properties more complicated
than for stable circular glass fibers. Cellulose is a hydrophilic molecule, so the
fibers have properties that are dependent on the water content. Fibers degrade
over time at temperatures of 200 0C or higher. Historically many fibers have been
used to reinforce various building materials. Recently scientific efforts have been
devoted to the use of natural fibers for reinforcement in cement-based building
materials.
Environmental conditions that occurred most recently led researchers to

try to get renewable materials that have a low environment impact. Utilization of
natural fibers as reinforcement in the design of building materials is an
opportunity to gain new and renewable construction materials. The use of fibers in
the material will reduce the impact on the environment. It will be highly beneficial
to the development of research on renewable building materials that do not affect
the environment and has reduced economic value.
Indonesia as a tropical country land has a significant amount of improving

coconut husk. It creates problems for the environment. Researchers are required to
describe the performance of coir fiber and its influence on the cement paste.
Reduction in the use of transport for materials will reduce the impact of
environmental emission. That condition inspired to use local materials. It needs
research to improve production and quality of local ingredients. Reduction of
greenhouse gas emissions and energy consumption required a decrease in the use
of cement and using natural and local materials. In the manufacture of building
materials establishment needs to get reliable results, quality, and quantity. The use
of extrusion technology is expected to overcome it. Literature review highlights
that there is a gap that needs to be filled by further research to provide mix design
methods for low cement content – natural fiber reinforced composites. Recent
developments published in the literature deals with the development of building
materials with low environmental impact. It can be done using reduced cement
content and natural fiber, especially the coconut fiber.
This research is a step to have profound insight to investigate the strength

of the bond between the coconut fiber and cement-based material because it then
contributes to a better behavior of the composite. The result of this work is helpful
in selecting the optimum fiber properties and pre-treatment to enhance the bond
44
between fiber and cement-based materials, ultimately resulting in increasing
strength of composites. The results of the state of the art, it is clear that research
has to be conducted to develop more of the characteristics and treatment of
coconut coir fiber in cement-based composites.
The construction industry is one of the major and most active. This
industry is also responsible for the depletion of large amounts of nonrenewable
resources and 30% of carbon dioxide gas emissions. The use of renewable
resources by the construction industry will help to achieve sustainable
consumption pattern of building materials. Development of building materials for
the construction, from the state of the renewable art research, should be continued
the formulation of materials with a low content of cement, improved local
materials and natural fibers as reinforcement. The formulation has a thermal
resistance as well as having a low environmental impact.
Furthermore, the process and production of the material can be evaluated

by using LCA software Simaphro. It has intended to assess the extent of the
environmental impact caused by the material. In this case, the result of the
evaluation is conducted on advanced research.
45
CHAPTER.3.
RESEARCH DESIGN AND METHODOLOGY
3.1. Introduction
The aim of this chapter is to describe the tested materials and the followed
experimental procedure. All tests are performed to evaluate the behavior of coir
fibers and both the rheological properties at the fresh state and the mechanical
properties at the hardened state of extruded coir fiber reinforced cement-based
composites. The first step consists in defining the materials used in the
experimental investigation and the testing devices. Methods and procedures are
explained in details. Experiments are conducted with the four following steps: 1.
The measurement of coir fiber strength; 2. The design of the fiber reinforced
cement-based composite; 3. Rheological characterization of the paste in the fresh
state; 4. Mechanical performance of the extruded composites at the hardened
state.
Furthermore, based on the results of the experiments, we can expect to

develop an analytical model able to describe the stress-strain of fiber cement
mortar composites
3.2. Flow chart of the experimental approach
This chapter describes the experimental approach and test procedures. The
raw materials used in this work are coir fiber and cement-sand-clay mixes. This
research design is summarized in Figure 3.1. The chart of the research work is
divided into three successive stages. The first one is the preparation research
carried out in the UI, Indonesia and continued at UBS, France. Then, the phase of
materials preparation and characterization is done in the laboratory at UBS,
France. This work performed in the laboratory that starts with the preparation of
materials consists of materials design and processing, followed by the physical,
mechanical and microstructural characterization. The last stage is analysis,
discussion and final conclusions held at UBS, France and UI, Indonesia.
46
At UI and UBS START
Literature Study
State of the art of building materials with low

environmental impact
Preparation research and submission theoretical
At UBS Research Methodology
Composition Preparation component materials Characterizatio

Composite and natural fiber treatment n Coir fiber
Rheology testing, Materials Processed by Extrusion Physical,

Microscopic And Molding Thermal,
observation mechanical,
Microstructure
Mechanical Testing
Yield stress model
Static Loading
By
Mechanical Testing System Digital Image Correlation (DIC)

(MTS) Non Destructive Testing
Destructive Testing
Macro-mechanical Failure Microstructure Damage Micro-mechanical

Performance Modes Composites Evolution Performance
Macro-mechanical Model Micro-mechanical Model
Discussion
At UI and
UBS Conclusions and Perspectives
END
Figure.3.1. The flow chart of the research design
47
As shown in the flow chart of research in Figure 3.1, the design and development
of material are organized as follows:
1. A selection of natural fiber and description of its extraction process.
2. The design of an extrudate mix of cement, sand and clay, reinforced by
natural fibers.
3. Effect of the fibers on the behavior of the cement paste at the fresh state.
4. Study of the physical properties of the material components using
morphological microstructure observations such as surface morphology,
shape, dimension using scanning electron microscopy (SEM).
5. Fabrication of extruded natural fiber reinforced cement pastes.
6. Measurement of splitting tensile strength and compressive strength of the
extrudates at the hardened state carried out simultaneously with
microstructure analysis by SEM observation
3.3. Fibers
3.3.1. Preparation of fibers
The used fiber is coir, which is a product from the coconut (Cocos
nucifera). The coconut trees are extensively grown in tropical countries. The coir
fiber of the present work comes from the island of Java Indonesia as shown in
Figure.3.3. Fiber has been extracted from coconut husks. In the present work, Coir
fibers are extracted manually from the coconut shell and outer membrane.
Cleaning and sieving steps are needed to obtain the fibers manually as
shown in Figure 3.2. After the coconut fibers are separated from the coconut shell
as shown in Figure 3.2.a, they are separated and released from peat that stacked
up into fibers (Fig. 3.2.b). Then fibers are sieved by length (3.2.c.d.e.f.). Residual
dust and peat are partially removed from fibers.
Two types of fibers are studied: fibers that are cleaned and thermally treated
and fibers that are untreated. Treatment of fibers is done manually without any
chemical additive. The cleaning consists in a washing of fibers with tap water to
obtain a smooth surface and to remove the rest of peat and dust that still exist on
the surface after sieving. Fibers are dived in clean water during 1-2 hours. Then
dirty water, loaded with peat and dust, is removed, and the operation is renewed
with clean tap water, to separate fibers. Some peats and dust are then extracted
manually from fibers skin and fibers are placed on a paper, so that it can absorb
water. Finally, fibers are combed and sieved, to release the residual peat and dust.
48
Those treated fibers are stored in a chamber at a 20°±1°C room temperature
before being put in the oven at 50˚ C for two days. The treated coir fibers are
shown in Figure 3.5. Untreated fibers are just left in an air-conditioned room
(temperature 20°±1°C and relative humidity of 50%), before tests. The untreated
fibers are shown in Figure 3.4.
a b c
g f
Figure.3.2. Extracted Coconut Fiber
The Fibers are carefully cut to the required length. After the drying of the
fibers room temperature, the long fibers were firstly separated from short fibers
and peat. Then three ranges of length were selected: 1 to 10 mm; 10 to 50 mm; 50
to 250 mm. All the fibers are then combed and finally cut to the required length
with scissors. Three lengths are studied: 5 mm, 10mm, and 15mm.
It must be noted that the coir fibers are also commercially available at
relatively high cost, as they are prepared for special purposes like brushes, mats,
and pedestal seats. This cost can be reduced if fibers are mechanically prepared at
a larger scale. Until now there has been no commercial product that provides
fiber-based uniform size and fiber size below 100 mm.
49
Figure 3.3. Coconut fibers.
Figure 3.4. Untreated coconut fibers.
Figure.3.5. Treated coir fiber
50
3.3.2. Water absorption
The water absorption coefficient was measured following the ASTM 127/88
standard. The untreated and treated fibers samples are weighed after drying at 50
o
C (until a constant weight is obtained). Then, the samples are immersed in
distilled water at a room temperature of 20 o C. The samples are removed from the
water after different immersion times and weighed with a high precision balance
and then dived again in water. A minimum of three samples was tested.
The weight difference provides the content of water. The absorption

percentage is calculated using Eq. (3.1).
.. (3.1)
3.3.3. Density tests
The density determinations for coconut fiber and coconut powder were
obtained by using the Archimedes principle. This principle states that any solid
object immersed in a fluid will lose weight an amount equal the fluid it displaces.
The laboratory METTLER TOLEDO balance is equipped for this experiment. At
first, the coconut fiber and coconut powder must be in a compacted form with the
diameter of 23.00 mm and thickness of 4.00 mm. After all the compacted
specimens have been prepared for both coconut fiber and coconut powder, the
second step was to measure the density of the compacted specimens by using the
balances. This device can calculate and give the density value automatically when
the specimens are put into the balances according to the setting that has been set
up. However, Equation 3.2 has also been used to calculate the density of the
specimens to compare the result of theory and experiment.
……………………….. (3.2)
Where: ρ is the density of sample, A is the weight of sample in air, B is weight of

sample in the auxiliary liquid, 𝜌 is the density of the auxiliary liquid, and 𝜌 L is
air density (0.0012g/cm3). Figure 3.6 shows the steps for density measurement
using Mettler Toledo balance device for porous solid. Procedure of density
measurements is as follow:
a. Setup the porous solid in the device,
b. Put the sample in the pan,
51
c. Dive the sample in oil and put it back in the pan,
d. Put sample in basket,
e. Compute the density value.
Figure 3.6. Density measurement using balances device.
3.3.4. Optical microscopy
An optical microscope is used for coconut fiber diameter measurements

before the mechanical tests (Figure 3.7). The average diameter is obtained after
the measurement of at least five measurements throughout the length of the fiber.
Figure.3.7. Optical Microscopy
3.3.5. Mechanical testing
52
The mechanical properties are an ultimate tensile strength, failure strain and
Young‘s modulus of single coir fibers. Those were determined using a universal
MTS tensile testing machine equipped with a 10 N capacity load cell. The device
used is the MTS Synergies RT/100 from the LIMATB laboratory. Bundle fibers
tensile strength is determined by applying a constant rate of displacement of 1
mm/min on a fiber length of 10 mm as shown in Figure. 3.8.
The tensile properties of the coir fibers were determined according to

ASTM D 638. Single fibers are manually separated from the bundles. Fibers are
cut into 40 mm length ones, and their diameters are determined used micro-optic.
Before testing, the fiber was glued to the paper frame. Its diameter is determined
by the average of optical measurements in minimal three different spots. Then, the
frame is clamped on the MTS machine. While mounting, the specimens were
handled using the paper frame. After the clamping of the ends of the paper frame
in the test machine, the paper frame sides were carefully cut in the middle, before
the start of the tensile test as shown in Figure. 3.9. The tests were displacement-
controlled with a loading rate of 1 mm/min at 20o C±1oC and 50% relative
humidity. The test was repeated 4 to 5 times, and the average values are reported.
Figure.3.8. Set up of the tensile test
Figure.3.9. Preparation of specimen for the tensile test
53
The MTS testing machine is used to determine the tensile strength of fibers.
This machine can plot automatic load versus extension graph. The fiber breaks
down automatically when it reaches its ultimate expansion. The point where the
fiber breaks down is known as the breaking point. From given data, stress and
strain can be calculated at breaking point from the load-extension data as follows:
……….…………………… (3.3)
……… …………………………(3.4)
The stress values (MPa) is calculated by dividing measured force values (N)
by the original cross-sectional area of the sample (mm2). Strain values were the
elongating part of the specimen in the percentage of the original length (L0 = 10
mm) while, young‘s modulus is determined as the slope of the linear part of the
stress–strain curve.
3.3.6. Scanning electron microscopy
To identify surface morphology of single fiber bundle samples and fracture

surfaces in the sample, a scanning electron microscope (SEM), type JEOL model
JSM-6460LV, was used (Figure 3.11). SEM produces high-resolution images of a
sample surface. It can resolve smaller feature, down to nearly 2 nm than a
standard microscope. The electrons lose energy by repeated scattering when the
primary electron interacts with the specimen. So absorption within a shaped
volume of the specimen known as the interaction volume extends from less than
100 nm to 5 nm into the surface.
54
Sample
Figure.3.10. Vacuum-system
Figure.3.11. Set up of Scanning Electron Microscope
The scanning electron microscope was used. The surfaces of the treated
single fibers and untreated individual coir fiber samples are examined and
observed at the acceleration voltage of 20 kV. The individual coir fiber samples
are mounted on stubs with silver paste. A thin film of platinum is vacuum
evaporated (Figure 3.10) to enhance the conductivity of the samples before the
photomicrographs taken with backscattered electron image and energy dispersive
spectroscopy (EDS). SEM images were realized to characterize the coir fiber, and
fracture surface made on samples tested in the tensile stress test.
55
3.3.7. Thermal gravimetric analysis
Thermo Gravimetric Analyses (TGA) were carried out using Mettler

Toledo equipment; Model TGA-50 attached to a Mettler TC 11 4000 thermal
analyzer as shown in Figure 3.12. The samples (10–20 mg) placed in platinum
pans and heated from 20o C to 1000 o C at the heating rate of 20 o C /min as shown
in Figure 3.13. The thermal analyzes were done in a nitrogen atmosphere at a
flow rate of 20ml/min. The synthetic air atmosphere was used to simulate the
usual conditions of the end use of this material. It yielded the onset temperature of
decomposition, mass loss, and maximum decomposition peak.
Figure.3.12. Thermogravimetric analyses device.
Figure.3.13. Thermo Gravimetric Analyses (TGA)
56
3.4. Fiber reinforced cement mortars, at fresh state.
3.4.1. Materials are tested.
3.4.1.1. Cement
The cement was a Portland cement CEM I/52.5 N CE CP2, from Lafarge
plant of Saint Pierre la Cour, France.
This cement was without any addition of mineral admixture or filler. The
cement size distribution, measured using a laser granulometry in ethanol, ranged
between 1 μm and 100 μm. The specific surface measured using a Blaine was
3,390 cm2 / g, and its density are 3,150 kg/m3. The chemical composition of
cement CEM I /52.5 N used as specified in the French Standard. It given in Table
3.1.
Table 3.1 Chemical composition of cement

Oxidations Proportion (weight %)
SiO2 22,40
Al2O3 2,85
Fe2O3 2,25
CaO 66,70
MgO 0,83
K2O 0,19
Na2O 0,17
SO3 2,20
CO2 1,30
CaO free 0,55
Insoluble 0,30
Alkaline 0,32
3.4.1.2. Sand
A graded river sand is used as fine aggregates. The raw sand used was a
Loire river sand, France. The river sand was used to mix the mortar according to
the ASTM standard C128, with a density of 2,600 kg/m3 and sand absorption
57
capacity of 2 %. The particle size distribution of the raw sand as shown in
Figure.3.14.
For extrusion formulations, sand particles were sieved under 2mm and then
ranged from 20 μm to 2 mm. Sand was stored in the laboratory and exposed to
fluctuating temperatures and relative humidity instability. Before mixing, Sand
was dried at 105 ° C for 24 hours.
Figure.3.14. Particle size distribution of sand
3.4.1.3. Water
The water used in this study was tap water, not subjected to any particular
preparation. Water was taken from the laboratory civil engineering LIMATB-
UBS in France.
3.4.1.4. Clay
The Clay/Kaolin used comes from the IMERYS quarry, located in

Ploemeur, France. It presents a density of 2,600 kg/m3. The chemical composition
of clay/kaolin is shown in Table 3.2. The SEM analysis of kaolin particles arises
in a laminated structure. Kaolin has a grain size ranging between 5 and 50 µm.
58
Table 3.2 Chemical Composition of Kaolin
Oxide Proportion (% mass)
Al2O3 48.15
Fe2O3 37.0
TiO2 0.8
CaO 0.1
MgO 0.2
K2O 1.1
Na2O 0.1
Li2O Traces
3.4.1.5. Super-plasticizer
Super-plasticizer was a High Range Water Reducing Admixture (HRWRA)

CHRYSO Fluid Optima 206. The HRWRA is a polycarboxylic type polymer. It is
in liquid form containing 20 % of the dry material. It recommended dosage ranges
from 0.3 to 3 % per weight of cement. In this study, dosage was fixed at 1.5 %.
Mixtures with an HRWRA were tested to estimate its efficiency to reduce water
content in fresh mixtures and to increase the strength of hardened mortars.
Table 3.3 Characteristics of CHRYSO Fluid Optima 206

HRWRA, CHRYSO Fluid Optima 206
Nature liquid
Density 1.05 ± 0.02
pH 7±2
Cl ¯ content < 0.1%
Na2O equivalent <1.0%
Dry 20.2 ± 1
Dosage 0.3 - 3 kg per 100 kg of cement
3.4.1.6. Natural Fibers
Fibers are described in Chapter 3.3. Coir fibers are added to most mixes.
Three different nominal fiber lengths are examined: 5 mm, 10 mm and 15 mm
(Figure. 3.15). The fibers were supplied as chopped strands that were made to the
individual fiber during the mixing operation (Figure. 3.16).
59
Figure 3.15. Coir Fibers Geometry
Figure 3.16. Chopped Coir Fibers
3.4.2. Mix proportion
The mix proportions are based on previous works done on cement stabilized
clay blocks [Khelifi et al., 2012]. Two mixes are studied. For lower cement
content, the cement proportion by mass was 10% of the total dry mix (mixture
without water). For higher cement content, cement was used at a mass dosage of
20% of the dry mix. For plain mortar, the mix contained mass ratios for cement,
sand and clay of 1:3:6 for low cement content. For high cement content of 2:2:6,
with water-cement (W/C) ratios by mass respectively of 0.21 and 0.19.
Three lengths of coir fibers are used: 5 mm, 10 mm and 15 mm The Coir
fibers contents were 2%, 3%, 4% and 5% by mass of cement.
The mix design for coir fiber cement mortar composites and water content
were the same as that of plain mortar. It is well known that the W/C ratio has an
influence on mortar properties, but compaction is also an important factor. The
60
addition of water will cause bleeding, ultimately reducing its strength in the
hardened state. Reduced W/C ratio can lead to improper compaction, and then can
result in less strength. Therefore, high range water-reducing admixture (HRWRA)
was used to achieve good workability. The HRWRA dosage fixed at 1.5 % per
weight of cement.
3.4.3. Mixing procedures
A standard Hobart mixer was used to mix the formulations. This device
provides a planetary motion and variable speed drives. Its volume capacity is 5
liters by EN 196-1 for the preparation of standard cement paste or mortar. The
mixer equipped with two rotation speeds 60 and 140 rpm as shown in Figure.3.17.
First of all, sand was mixed with fibers then blended at a mixer speed of 140
rpm (0.37/s) for 5 min. This step is followed by a 60 s at rest for bowl scraping.
The second step consists in pouring cement and clay/kaolin and mixing the batch
for 3 minutes. Then tap water was added while mixing again for 6 minutes at 280
rpm (0.74/s). The composite mix is stirred manually to disperse fibers in the
matrix.
Figure. 3.17. Hobart mixer
3.4.4. Rheometer tests
61
The rheometer test is a vane test that allows to study the rheology of
viscoelastic or plastic materials. It is suitable for perfect plastic materials and
leads to the formation of a homogeneous stress state along the fracture surface
defined by the movement of the tool.
At constant and low rotational velocity, the rheometer measures the value of
the stress at break under shear and normal stress to zero on a facet of rupture. This
stress is called yield stress and is usually denoted by 𝜏o. It is noteworthy, that the
tool inserted into the mortar does not cause damage. The resistance to movement
of the material induces a torque on the motor shaft. The passage of torque to shear
stress is achieved by setting the time when the sum of torsions induces shear
stresses acting on the sheared surfaces. This results in the relationship between
torque and shear stress,
𝜏o …………..………….…….………. (3.5)
Where, 𝜏o = Shear yield stress; T = torque; B = constant dependent on the
geometry. In this case, the tool is pressed into the sample to a depth corresponding
exactly to the height H of the blades. Geometry sheared is that of the cylinder of
height = H and a radius = R.
………………………………………. (3.6)
………………………………………. (3.7)
In addition, the Rheometer is used in the present work as a tool for the
formulation of extrudate paste. It is based on the criteria established for
cementitious material by Toutou et al. [Toutou et al., 2005]: The pastes should
have a yield stress around 20 kPa.
To measure the yield stress, we use an Anton Paar Rheolab QC rheometer

equipped with vane geometry as shown in Figure 3.18. The vane geometry
utilized in this study consists of four blades around a cylindrical shaft. The blade
height is 8.8 mm, and its diameter is 10 mm. Tests were conducted at very low
speed (0.01 rad/min). At such a low shear rate, viscosity effects are negligible,
and yield stress can compute from the measured torque peak value at flow onset.
The experiment procedure is similar to the one used in Mahaut [Mahaut et al.,
2008].
The tests are conducted at imposed strain rate. The rheometer worked like a
current one but was controlled by a microcomputer: it can operate at constant
62
speed or constant torque. The dimensions of the tool is known, the torque values
are directly converted into shear stress.
Figure 3.18. The Anton Paar Rheolab QC Rheometer
3.4.5. Screw Extrusion
The used extruder is a single screw extruder for horizontal extrusion Type
VAVRS 50 with a Barrel diameter of 50mm and Max. Pressure rate 150 bar. The
diameter of the auger is 48.5 mm. The total installed power is 4.4 kW. The device
is shown in Figure.3.19.
Implementation of material flow is provided by a rotating screw in the arm

commonly called cylinder extruder body. To reduce the amount of air entrained in
the product formed, the vacuum pump can be easily incorporated the system,. The
extruder forcing the paste flow through a die and the mix undergoes high-pressure
gradient that makes its structure matrix very compact (low porosity).
The cement paste that comes out through the extruder must be
simultaneously stiff enough to hold its shape through the die area and sufficiently
flexible to limit the power of processing. Both conditions are fulfilled when
cementitious materials exhibit an optimum yield stress of 20 kPa [Toutou et al.
2008]. Specimens of suitable dimensions are cut using a diamond cutter for
mechanical testing as shown in Figure.3.20. Most care has been taken to maintain
uniformity and homogeneity of the composite.
63
Figure.3.19. Screw Extrusion
Figure.3.20. Cutting extruded the mortar
3.4.6. Casting procedure
The plain mortar and coir fiber-reinforced mortar composites are mixed in
a mortar mixer. Fresh concrete workability was investigated immediately after the
final mixing of the mortar using the rheometer. Then the mixture was poured into
molds. It as shown in Figure 3.21 for the cylinder.
64
Figure.3.21. Cylinder sample
Figure.3.22. Vibrating of cylinder
The cylinder was cast by filling each mold in four layers. Each layer had
frequently been compacted with 25 blows from a wood rod of 16 mm diameter
before the next layer was poured, and the vibrator used. A plate vibrator is used to
avoid entrapped air in the mold. Those cylinders were cast and vibrated on a
vibrating table without pressure and cured in a wet chamber until the date of the
test. All the samples are cured for 28 days before testing.
3.5. Fiber reinforced mortar composites at hardened state.
After a fiber tests and rheology test performed at fresh state, other
experimental tests such as compressive strength, tensile splitting strength tests,
and SEM observation were carried out on all of the hardened samples.
3.5.1. Specimens preparation
Preparation of the test samples is shown in Figure 3.23: mortar cylinders of

35 mm in diameter and 70 mm in height for screw extrusion were tested. Those
tests are carried out for both plain and coir fiber-reinforced mortar composites for
the determination of different properties of mortar/ matrix. The mix proportion of
1:3:6 and 2:2:6 by the weight of ordinary Portland cement, clay/kaolin, river sand
and coir fiber were used to cast the specimens. The water/cement ratio used is
0.19. The water/cement ratio was maintained constant at all different length and
volume fraction of fibers.
65
All samples were left in the molds for 24 hours to set at ambient
temperature. They were removed from the mold and transferred into a curing in
the air and immersion tank. The curing temperature was 20±1°C and humidity of
approximately 50% ± 5%. The concrete mixes and the specimens are prepared by
the provisions of EN196-1 standards. Then mechanical tests were carried out after
7 and 28 days of curing.
Figure.3.23. Sample cylinder of test
3.5.2. Water absorption.
The Samples were dried in hot air oven at 55 o C until their weight was
constant.(Wi). Then, they were immersed in 50 ml distilled water. The swollen
samples were wiped and weighed (W W) after 24 hours. Then, they were dried in
hot air oven at 55 o C until their weight was constant (W f). Each sample is
analyzed in four replications. The water absorption formula is as follows:
Water absorption (WA) = [100 x (W w – W f) / (W i)] (%) ……… (3.8)
3.5.3. Density tests.
The density of plain and coconut fibers reinforced mortar: The weight and
volume of plain and fibers reinforced mortar were measured before the
compressive strength test.
The theoretical density of composite materials in terms of the weight

fraction can easily be obtained from the equations (3.9):
(3.9)
66
ρ is density and W are the weight fraction respectively. The suffix f is fiber; m is
matrix and ct are the composite materials.
The actual density (ρ ce ) of the composite, however, can be determined

experimentally by simple water immersion technique. The volume fraction of
voids (V v) in the composites is calculated using the following equation:
(3.10)
3.5.4. Compressive tests.
Compressive strength test of plain and coir fibers mortar composites were
carried out to find the modulus of elasticity, compressive strength, and finally to
observe the stress-strain curves. The modulus of elasticity (E) is calculated as the
ratio of stress change to strain change in the linear elastic range of the specimens.
The maximum value of stress in stress–strain curves taken as the compressive
strength (σ), and its corresponding strain (ε) is also noted.
The INSTRON 8803 testing machine was used to determine compression
strength of the plain concrete and coir fiber cementitious composites. This
machine can plot a graph of load vs. time automatically. The loading capacity of
this machine is up to 500 KN. The experiment has been done using a compressive
rate of 0.00015 mm sec-1. Mechanical tests were performed following European
standard EN 196-1 prescriptions [European standard, 2000]. The
experimental compressive strength test was done in the laboratory as shown
in Figure 3.24.
Figure.3.24. Cylinder Axial Compression Test
67
3.5.5. Tensile tests
The tensile test is performed on the Instron type 8803 (Instron, USA) testing
machine at a crosshead speed of 5 mm/min, using a 50 KN load cell. The
maximum load from the load-time curve of the splitting tensile strength (STS) test
is taken for the calculation the tensile strength of plain/mortar and composite
samples.
In splitting tensile strength test, cylinder sample exposed compressive force

along the direction of the long cylinder. The resulting orthogonal tensile force
causes the sample to fail in tension. The tensile splitting strength is calculated by
using the following equation:
...................................................... (3.11)
Where f ct is the tensile splitting strength, in MPa, F is a maximum load of N, L is

the length of the specimen in mm, d is the cross-sectional diameter, in mm.
Figure.3.25. Tensile test setup
3.5.6. Digital image correlation
The Digital Image Correlation (DIC) system is a method for identifying

the distribution and development of strain without the need for direct sample
contact. the displacement of a sample of an applied speckle pattern coated on the
surface is tracked on the basis of pixel distortion before converted into a measure
of strain, using high-resolution image capture.
68
The DIC method works by correlating the digital images of surface
patterns before and after straining. It consists of a three dimension digital image
correlation (3D-DIC) system, sensor ARAMIS 4M, and computer. The 3D-DIC
setup consists of two cameras having a max frame rate 60 Hz at a spatial
resolution of 2358 x 1728 pixels, coupled with Titanar lenses of 35 mm length.
Both cameras are mounted on a tripod having inbuilt spirit level to ensure
horizontal level. Mechanical Testing System (MTS) Instron 8803 machine of 500
kN capacities as controlled. A typical experimental setup used in the present study
as shown in Fig. 3.26.
Lighting
Sample
DIC Cameras
DIC Cameras
MTS Machine
Load
Cell User interface for MTS
Image grabbing system
Figure.3.26. Digital Image Correlation and Testing Setup
In preparing the samples for DIC, a black-on-white speckle pattern was

applied to the prepared surface. Random speckle patterns are made over the
sample surface by spraying carbon black/titanium white colors with an airbrush
69
having a nozzle diameter of 0.5 mm. The test recorded images are then uploaded
to the evaluation software ARAMIS and calibrated. Initial widths of the samples
were measured pretest using an optical microscope. Two cameras were mounted
on a tripod and profile bar then centered symmetrically about the sample position.
Uniform illumination of the specimen surface is ensured by keeping two

standard halogen light sources on either side of the camera. The surface of interest
is zeroed on by adjusting the focal length of both the lenses. The aperture of the
lenses is adjusted to achieve a proper field of view and also to avoid saturation of
the pixels in the area of view. The camera then calibrated for its position and
orientation using an appropriate calibration grid plate. Cameras are connected to a
workstation computer, and the images grabbed at a predefined rate.
The real-time results for multiple measurement positions the test objects
surface directly transferred to the testing device, data acquisition units. Data
acquisition card is used to provide an interface between MTS controller and image
grabbing system for storing the required data like load and displacement values
for every image being grabbed.
3.5.7. Microscopic observation.
The microscopical analysis in this study based on scanning electron

microscopy (SEM), with backscattered electron image. Backscattered electron
imaging is appropriate for sectioned specimens with a smooth, polished surface.
The scanning electron microscope JEOL JSM-6480LV (Figure 3. 11) used

to identify the tensile fracture morphology of the coir fiber cement the mortar
composite samples. The surfaces of the composite sample observed at 20 kV
acceleration voltage. The composite samples mounted on stubs with silver paste.
A thin film of platinum is vacuum evaporated onto them before the
photomicrographs taken to enhance the conductivity of the samples, as shown in
Figure 3.10.
70
CHAPTER.4.
PHYSICAL, MICROSTRUCTURE, THERMAL AND
MECHANICAL PERFORMANCES OF COIR FIBERS
4.1. Introduction
Recently, research on green building materials becomes a way to

anticipate global warming issues. Among these researchers, development of
natural fibers as a concrete reinforcement is an emerging topic. The amounts of
natural fibers such as coconut fiber materials are abundant in Indonesia. Coir fiber
is a residual product of the copra (coconut meat) production, with volumes that
exceed the needs for traditional uses like cords, brooms, Etc. Coconut fibers have
the potential to be used in composite materials as reinforcement. This study deals
with the description of the properties of those natural fibers from Indonesia.
The proposed methodology is to perform experiments to observe coconut

fibers with and without special treatment (here a simple water washing followed
by a dry stage). Mechanical properties were investigated through fibers direct
tensile tests; Physical and thermal properties were studied using thermal
gravimetric analysis. Finally, micro-structural properties fibers were obtained
using a scanning electron microscopy (SEM).
In this research, a water washing treatment is used to modify the

Indonesian coconut fiber surface. This treatment consists in a surface washing
with water followed by a drying stage. No work has been reported on the
treatment of Indonesian fiber surfaces. The effects of surface treatments of
coconut fiber on microstructural and mechanical tensile tests of coconut fiber
were investigated to assess its effectiveness.
The distribution of the tensile strength is studied, the mean and standard
deviation of tensile strength is calculated following the Normal distribution and
Weibull distribution resulting in the questionable benefit of applying the Weibull
distribution.
71
4.2. Physical properties
The physical properties of any natural fiber are important to describe the
mechanical strength of the fibers. Physical properties should include fiber
dimensions, defects, strength, variability, crystallinity, and structure. It is
important to describe the physical and mechanical properties of the fibers to
optimize their potential as reinforcement in a cement matrix.
In order to optimize the efficiency of fibers in cement composites, it is

necessary to carry out the treatment by washing and drying coir fiber in order to
extract the substances responsible for the possibly weak interaction between fibers
and cement mortar.
Treatment of fibers is done manually without any chemical additives. The

present method of treatment is made through a process of washing and drying.
After one day storing period in an air-conditioned room at 20°±1°C, fibers are
soaked in tap water for two hours. This immersion sequence is repeated twice.
Fibers are separated from dust and peat by sieving and combing. Then, fibers are
cut in 5mm, 10mm, and 15mm long fiber bundles. Finally, fibers are dried in an
oven at 50°C for two days. Figure 4.1 shows untreated coir fiber, and Figure 4.2
presents treated coir fiber.
Figure. 4.1. Untreated coir fiber

Figure.4.2. Treated coir fiber
4.2.1. Length of coir fiber
The natural length of coconut fibers ranges from 40-250mm. The lengths
of fibers were measured using a steel ruler, and 50 pieces were randomly chosen
72
to find out the length distribution of coconut fiber. However, in this study,
coconut fibers are cut in 5 mm, 10 mm and 15 mm fiber bundles.
4.2.2. Diameter of coir fiber
Changes in the physical properties can be due to differences in fiber

morphology. Major differences in a structure such as density, cell wall thickness,
length, and diameter result in different physical properties. Knowledge about
diameter is important in cellulose based fiber composites as it give an indication
of possible strength properties.
Treated coir fibers are cut into 40 mm long samples and their diameters
are measured using an optical microscope. The cumulative distributions of fiber
diameters are shown in Figure 4.3 for both treated and untreated samples. Fiber
diameters distribution is modeled using an exponential based models as shown in
the equation (4.1) for untreated fibers (mean square error coefficient R2 is equal to
0.9716) and equation (4.2) for treated fiber (mean square error coefficient R 2 is
equal to 0.9578).
Duff = 77.065 e 0.0064 F ………………...... (4.1)
Dtf = 55.423 e 0.0046 F ………………...... (4.2)
Figure.4.3. Diameter of untreated and treated coir fiber
73
The cumulative diameter distribution of fibers is modeled for composite
materials with Weibull model. The cumulative distribution of the diameter of
treated coir fiber is shown in Figure 4.4. The average value of fiber diameter is
106.56 μm for treated fibers with a standard deviation of 37.12 μm. The
cumulative distribution of treated coir fibers diameter is described by Equation
(4.3).
………………………….(4.3)
Figure.4.4. Diameter cumulative distribution of treated coir fiber by the two-

parameter Weibull
The cumulative distribution of the diameter of untreated coir fiber is

shown in Figure 4.5. The average value of fiber diameter is 154.99 μm for
untreated fibers with a standard deviation of 60.13 μm. The cumulative
distribution of treated coir fibers diameter is described by Equation (4.4).
………………………….(4.4)
74
Figure.4.5. Diameter cumulative distribution of untreated coir fiber by the
two-parameter Weibull
4.2.3. Density of coir fiber
The density of each fiber is an important parameter. For composite

materials, the density of fiber has a significant effect. The weight of fiber in a
composite matrix depends on the density of fiber.
The density of coir fibers was calculated using Equation (3.2).The density
of untreated coir fiber is measured at 878 kg.cm-3. For treated coir fibers, the
density is 980 kg.cm-3. . The difference between treated and untreated fibers
densities can be explained by the removing of pith and low-density impurities
(wax, dust) located at the surface of the fibers during the washing treatment.
Empirical equations (4.3) and (4.4).for density of untreated fiber and

treated fiber are found by a numerical fitting on experimental results as shown in
Figure 4.6. It can be observed that density increases with the fiber bundle length.
For untreated fiber, the mean square error coefficient R2 is equal to 0.9125,
uf = 0.1492 ln (Lf) + 0.1339 ……….…………………… (4.3)
For treated fiber, the mean square error coefficient R2 is equal to 0.9909,
tf = 0.1339 ln (Lf) + 0.353 ……………………………… (4.4)
75
Figure.4.6. The density of untreated and treated coir fiber versus fiber length.
4.2.4. Water absorption of coir fiber
During the mixing and drying of matrix cement or mortar, natural fibers
can absorb water and expand. The swelling of the fibers pushes away the cement
matrix, at least at the micro scale. At the end of the fibers drying process, fibers
have shrunk and are almost back to their original size. This phenomenon may lead
to the void creation and very low-quality interfacial bonds between fibers and
cement matrix. Therefore, it is necessary to measure the water absorption of fiber.
The measurements of absorption were carried out for 24 hours.

Experimental data have shown that the absorption rate of water by coir fibers is
maximal during the first three minutes. The absorption rate then drastically
decreases. After two hours of immersion, the fibers get almost fully saturated. The
absorption coefficient (ratio of the water mass over the fiber mass) is 82.4 % for
treated and 120.9 % for untreated as illustrated in Figure 4.7. The amount of
absorption is close to the one proposed by Savastano et al. (93.8 %) [Savastano et
al., 2000].
This difference between treated and untreated fibers may be explained by

the removing of dust, pith, and wax at the fiber surface. Those elements present a
high specific surface that need at least to be wetted during the absorption
measurement.
76
Figure.4.7. Water absorption of coir fibers
4.3. Microstructure analysis
The microstructure analysis was based on scanning electron microscopy

(SEM), with backscattered electron image and energy dispersive spectroscopy
(EDS). Examination of the fracture surface morphology of fibers and fiber surface
by using these tools will provide accurate observations.
4.3.1. Surface morphological characterization

The morphology of the fiber and their diversity of size are shown to
characterize coir fibers obtained after manual selection. Figure 4.8 showed the
micro-optical observation of both untreated and treated coir fibers bundle.
Untreated coir fibers apparently contain impurities such as wax, fatty substances
and globular protrusions [Rout, 2000]. There were significant differences in the
fiber morphologies after treatment compared to untreated ones.
77
Figure.4.8. Untreated (A) and Treated (B) of coir fibers.
It is observed that treatment makes the fibers cleaner and reduces their
surface roughness with almost all impurities removed from the fiber surface. The
treatment removes wax and cuticles at the surface resulting in a smoother
interface. Figure 4.9 shows the SEM micrograph of the untreated raw coir fiber
bundle. The fiber surface appears to be smooth due to the presence of waxes and
oil. However, the presence of pores could be seen on the surface. It shows a rough
surface where hemicellulose, lignin and natural wax substances still stick on the
surface [Li, Wang and Wang, 2007; Wang and Huang, 2009; Asasutjarita et al.,
2009]. On the other hand, treated fiber has a clean and smooth surface as shown in
Figure. 4.9. B. Longitudinal depression becomes apparent at the surface
[Lumingkewas et al., 2012b]. Coir fibers have a relatively smooth surface (Figure
4.9B), which can suggest a possible poor interaction between the fibers and the
matrix.
Figure.4.9. Micro-optic of untreated (A) and treated (B) single coir fiber
Morphology of untreated coir fiber and treated coir fiber are shown in
Figure 4.10 with three different sizes magnitude (x100, x300 and x1000) using the
SEM micrograph. On the surface of the untreated coir fiber, particular silica
groups represented by white dots are found.
78
These silica crystals have formed in the locations of the interaction between the
surface of the fiber and the pith of coconuts. On the other hand, the SEM
micrograph of coir fiber after treatment there was a reduction in the silica particles
as shown in Figure 4.25F at x1000 magnification. The removal of surface
impurities on coir fibers is advantageous for fiber–matrix adhesion as it facilities
both mechanical interlocking and the bonding reaction.
The morphological characterization provides useful information on the

characteristics of fiber surface and internal structure, which will be helpful in
predicting fiber interaction with the matrix [Castro et al., 2012].
Figure.4.10. SEM micrograph of surface untreated coir fiber (A. x100; B

x300; C. x1000) and treated coir fiber (D. x100; E. x300;
F. x1000).
79
4.3.2. Energy dispersive spectroscopy analysis.
SEM observations on treated fibers show small white protrusions or

bumps on the surface. EDS (Energy dispersive spectrometry) analysis tells us that
these white bumps present dominant silica content as illustrated in figure 4.11;
4.12 [Lumingkewas et al., 2012a]. SEM observations of other white bumps with
the little amount of silica are shown in Figure 4.13; 4.14. The amount of oxygen
represents the largest percentage of mass for both treated and untreated fibers. The
results of the chemical composition of coir fiber in the spectrum of 1 and 2 using
EDS are shown in Table 4.1; 4.2. EDS analysis of the chemical elements of the
white dots is shown in Figure 4.15. They mainly consist of carbon, silica and
oxygen.
The natural fibers are mainly built of cellulose, hemicellulose, lignin and
wax. Those elements consisted of carbon, oxygen and hydrogen elements. In the
general case, high electron intensity of carbon and oxygen are detected while that
of others substances like siliceous, potassium, sodium, magnesium, calcium, iron,
aluminum, sulfur and phosphorus are also found in smaller quantities [Jústiz-
Smith et al., 2008]. In the present case, only siliceous is found among those other
elements.
Figure.4.11. The surface of treated fiber with the white dots spectrum 1
80
Figure.4.12. EDS analysis of the white dots spectrum one characteristics
Table 4.1 Chemical composition of Coir Fibers at Spectrum one by EDS
Element Mass (%)
CK 20.09
OK 53.25
Si K 24.77
Ca K 0.35
Cu L 1.55
Total 100.00
81
Figure.4.13. The surface of treated fiber with the white dots spectrum 2
Figure.4.14. EDS analysis of the white dots spectrum two characteristics

Table 4.2 Chemical composition of Coir Fibers at Spectrum two by EDS
Element Mass (%)
CK 44.10
OK 40.26
Si K 13.10
Ca K 0.90
Cu L 1.63
Total 100.00
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Figure.4.15. EDS analysis of the element chemical of the white dots
characteristics
4.3.3. Fracture surfaces observations.
Scanning electron microscopy was used to examine the fracture surface

and the polished surface of fibers and fractured fibers morphology as shown in
Figure 4.16 for untreated coir fiber, and 4.17 treated coir fiber cross-sections. The
images of the internal morphologies of the coir fibers reveal a hollow porous
structure. Fiber pores are smaller after treatment. That leads to the measurement
of fiber diameter nearly 20% smaller than the one of the untreated fibers (Figure
4.18).
These images show different surface morphologies. It also shows images

of sections of various fibers (Figure 4.16) to characterize fibers cells and to
compare them with those observed in the literature. It appears that studied fibers
represent bundles of glued individual fibers (here the cells). These two images
83
were chosen to show the section of coir fiber at different scale magnification. The
first, Figure4.16 at this scale x 100, we can see the cells of the fiber and air gap in
their center.
In the second image is shown after x1000 magnification (Figure 4.17), the
section of the fiber at a major scale is observed and allows seeing with more
details the different cells of the fiber. We can see the wall of one of the cells of the
fiber that has been extracted during the fracture of the fiber.
The fractured cross section obtained after the fiber tensile strength test is shown in
Figure 4.19 using the SEM micrograph. In one fiber bundle, there are several
single fibers in the form of a spiral. These spiral fibers induce large elongation at
break and can explain the ductile properties of coir fiber bundles.
Figure.4.16. SEM image of cross-section of a typical coir fiber at x100
84
Figure.4.17. SEM image of elementary fibers which show different lumen
and cell wall of coir fiber at x 1000.
Figure.4.18. SEM image of cross section of treated coir fiber at x500
85
Figure.4.19. The SEM micrograph of the cross section of treated coir fiber at
x500 after tensile stress
4.4. Thermogravimetric analysis
The results of thermogravimetric analysis (TGA) for untreated and treated

coir fibers are shown in Figure 4.20and Figure 4.21. TGA curve, DGA
(Derivative of TGA) curve, and Heat Flow curve result are summarized in Table
4.3.
The thermal resistance of the fiber is affected by its chemical content.

Coconut fibers are characterized by higher lignin content and consequently
stronger aromatic properties [Frollini, 2013]. The chemical characterization of the
fibers, as expected, present three major components (known as natural fibers)
which are cellulose, hemicellulose and lignin [Fengel et al., 1984]. Deviations
from literature [Satyanarayana et al., 2007] could depend on several factors such
as soils, weather conditions during growth and harvesting and harvesting time.
Many other factors could affect the fiber composition as pre-treatment performed
during harvesting or extraction of the primary product [Sousa et al., 2004].
The TGA curves of the heat is treated fibers under nitrogen atmosphere
also exhibited a similar pattern than the TGA curves of untreated coir fibers
86
reported in the literature [Tomczak et al., 2007] and performed under an oxygen
atmosphere.
Table 4.3 Thermogravimetric results for coir fibers

Coir fiber Transition Temperature Weight Residual
temperature of maximum Loss Weight
range rate of weight (%) (%)
(°C) loss (°C)
Untreated 30 - 130 84.07 7.93 92.03
130 - 280 278.45 18.36 73.67
280 - 750 344.33 74.19 25.47
Treated 30 - 130 71.57 4.10 95.87
130 - 750 344.17 72.13 23.74
Figure 4.20 TGA curves of the heated untreated coir fibers under nitrogen
atmosphere
87
Figure 4.21 TGA curves of the heated treated coir fibers under nitrogen
atmosphere
4.4.1. Residual weight
The initial weight loss with the temperature ranging from 30 °C to 130 °C
is due to dehydration and can be considered beneficial to processing as it makes
the fiber more flexible and easy to buckle [Ndazi et al., 2006]. The residual
weight of coir fibers is strongly decreased for temperature ranging from 130 °C to
280 °C. Then, from 280 °C to 800 °C the residual weight slightly decreases.
Figure 4.22 shows the TGA of treated and untreated coir fibers under a nitrogen
atmosphere.
Figure 4.22. TGA curves of the heated treated and untreated coir fibers
under nitrogen atmosphere
88
The increase in thermal stability has been associated with an increase in
stiffness of the fiber and a decrease of amorphous hemicellulose. Condensable
components responsible for the fiber plasticization can also be the reason for the
large decrease in tensile strength and elongation at break, but also of the high
sensitivity of the materials to temperatures and durations of heating. Thermal
stability is influenced by chemical interaction within the fiber; it can be linked to
the effect of the heating on the tensile properties of the fiber.
4.4.2. Derivative weight
To evaluate the thermal stability of the coir fibers, TGA is performed.

Then, TGA and DGA curves are reported in Figure 4.23. TA-software is used to
obtain the derivative of TGA curves (DGA).
Thermal decomposition parameters were determined from the TGA curves

at a heating rate of 20 °C/min. In the present study, decomposition of the
untreated coir fiber shows several stages, indicating the presence of various
components that decompose at different temperatures. Due to the differences in
the chemical structures of lignin, cellulose and hemicellulose they usually
decompose at different temperatures. The degradation processes occur
successively to water desorption, hemicellulose, cellulose, and lignin.
In this study, a small weight loss was found in the range of untreated 30
°C to 70 °C and treated 30 °C to 50 °C due to the evaporation of water or low
molecular weight compounds. At approximately 50–70 °C all fibers present 2–3%
of weight loss due to the absorbed water [Paiva and Frollini, 2006; Megiatto et al.,
2007]. Moreover, they are thermally stable up to 130–250 °C, which can be
considered to be the maximum processing temperatures because of the negligible
weight loss. At higher temperatures, hemicellulose decomposition occurs at 150
°C to 280 °C followed by cellulose degradation at 280 °C to 350 °C. Lignin starts
to deteriorate at approximately 350 °C to 750 °C, due to cleavage of aromatic
rings and generation of several products such as water, methane, carbon monoxide
and carbon dioxide [Megiatto et al., 2007]. This process occurs in a wide
temperature interval due to the involved degradation of lignin with respect to
cellulose and hemicellulose since lignin presents a reticulated structure [Tomczak
et al., 2007].
The DGA shows that untreated coir fiber with the degradation of the
cellulose component degrades at 300 °C, and lignin begins its thermal
decomposition at 350 °C and persists until 750 °C. These results are similar to
other natural fibers as reported in the previous article [Abraham et al., 2013].
89
Here the degradation of treated cellulose exhibits an upper value of 354 °C
which slightly differs from the cellulose embedded in the untreated coir fibers
(338 °C). This reduction in the degradation temperature is due to the presence of
strong lignin–cellulose complex that exists in raw coir fiber. Raw coir fiber has a
lignin content of 45–50% of weight [Abraham et al., 2013].
Figure 4.23. DGA curves for the heated treated and untreated coir fibers
4.4.3. Heat flow
Heat flow for untreated and treated coir fibers are presented in figure 4.24.
Treated coir fiber heat flow is more stable than for untreated coir fiber. The
transition temperature of coir fiber ranges from 30 °C to 750 °C.
The increase in thermal stability has been associated with an increase in

stiffness of the fiber and loss of the amorphous hemicelluloses. On the other
hand, no condensable components responsible for the fiber plasticization can also
be the reason of not just considerable decrease of tensile strength and elongation
at break but also of the high sensitivity of the properties to temperatures and
durations of heating. Thermal stability is influenced by chemical interaction inside
the fiber and can be linked to the effect of heat treatment on the tensile properties
of the fiber.
90
Figure 4.24. TGA curves of the heated treated and untreated coir fibers
under nitrogen atmosphere
4.5. Mechanical properties
Means of tensile tests obtain mechanical properties carried out on single

fiber bundles. They are performed to get the tensile strength, the elastic modulus
(in the linear part) and the elongation at break. These values were compared for
untreated and treated samples to assess the treatment influence on the mechanical
properties of coir fibers.
4.5.1. Tensile strengths
Single fiber tensile properties are critical for the efficiency of fibers to be
used as reinforcement in concrete composites. These fibers properties directly
affect the behavior of the composites. Given mechanical properties, treated
coconut fibers present better tensile strength compared to untreated ones. Typical
tensile stress versus strain of coconut fiber is shown in Figure 4.25. For the tested
size of 50-99 mm in diameter, differences are significant between treated and
untreated fibers. Treated fibers have about 87.4% higher tensile strength and
119.4% more failure strain. Tensile test results show that fibers behavior is linear
elastic until the axial strain reaches 0.03 (mm/mm). Then, the fiber behavior loses
is linearity and the fibers finally broke. The strain failure value of 0.62 shows the
ability of the coconut fibers to exhibit ductile behavior.
91
Figure 4.25. Tensile stress vs. strain curve of the coir fiber
Partial vanishing of wax, hemicellulose and lignin on the surface of treated

fibers has led to higher fiber tensile strength [Hemsri et al., 2012]. Besides
pretreatment contributed to higher strength, this partial vanishing of surface
impurities allowed for a better and more homogeneous distribution of stress along
the fiber diameter. It states that the coconut fibers present an extremely ductile
behavior. This result has also been obtained in previous works on the same topic
[Munawar et al., 2007; Li Z., 2007; Rao and Rao, 2007]. The tensile properties
measured in the present work are in agreement with various earlier investigations
[Romildo, 2005].
Figure 4.26 illustrates the effect of the fiber diameter on the tensile
strength of coconut fibers. It can be seen that the diameter of 100-149 micrometer
gives the highest tensile strength values than other diameters. That can be
attributed to the fiber brittleness and defects caused by the coconut growth for
diameter higher than 150 m.
From the tensile test results for treated and untreated fibers, it appears that
there is a correlation between fiber diameter and tensile strength. Equation gives
formulation for untreated fibers (4.5):
4 3 2
σf = -11.429Df + 161.68 Df - 797.32 Df + 1568.1 Df - 845.7 ..... (4.5)
While the formula for the treated fibers is given by equation (4.6):
σf = 13.2 Df 4 + 191.83 Df 3 - 963.7 Df 2 + 1916.5 Df - 1033.9 .....(4.6)
Where σf is the tensile strength and Df is the Diameter of fiber.

Figure 4.26 confirms that treatment of fibers increases the tensile strength of
coconut fiber whatever the fiber diameter is.
92
Figure.4.26. Diameter versus Tensile strength of untreated and treated coir
fibers
4.5.2. Young’s modulus
The Young's modulus is plotted in Figure 4.27 as a function of the

diameter of coir fibers. The large distribution of the measuredYoung's modulus
may be due to the cross section of coconut fibers are not perfectly circle, but
ellipsoidal. Moduli of elasticity for the untreated fibers were found to range
between 1 and3 GPa. While treated fibers exhibit elastic moduli ranging from 2
to6 GPa. These values are in the range reported in the literature for the diameter of
100-149 µm, [Tran LQN et al., 2014], [Ali M et al., 2012], [Defoirdt N et al.
2010], [Li et al., 2007], [Toledo et al., 2005].
From the tensile test results for treated and untreated fibers, it appears that
there is a correlation between fiber diameter and Young‘s modulus. For untreated
fibers, the Young modulus evolution is well described by Equation (4.7):
4 3 2
Ef = -0.1455Df + 2.0252 Df – 9.8395 Df + 18.936Df - 9.732 ..... (4.7)
While for treated fibers, the Young modulus evolution is well described by
Equation (4.7):
Ef = 0.311 Df 4 + 4.2982Df 3 – 20.879Df 2 + 40.685Df - 22.29 .....(4.8)
Where Ef is the Young‘s modulus and Df is the Diameter of fiber.
93
Figure.4.27. Diameter vs. Young’s modulus of coir fibers
4.5.3. Elongation at break
The elongation at break (ε) of untreated and treated fibers versus their
diameters is shown in Figure 4.28. Elongations at break of the treated fiber are
higher than the untreated fibers ones for the same diameter. Also, it seems that
there is a linear relationship between elongation at break and fibers diameter.
The graph in Figure 4.28 gives the evolution of elongation at break

regarding the fibers diameters. This evolution of elongation at break can be
written as follow for untreated fibers with R² = 0.9793:
ε = 10.53 Df + 20.23 ………………………………………………(4.9)
The same type of equation can also be written for treated fibers with R² = 0.9437
ε = 12.059 Df + 26.25 ……………………………………………(4.10)
94
Figure.4.28. Diameter vs. Elongation at break for coir fibers
The mechanical properties of treated and untreated coconut coir fibers are
reported in Table 4.4. It presents the results of coco fiber from other countries
without reference to the size or diameter of the fibers. Indonesian coir fiber has
the highest value of elongation at break. Similarly, the values of tensile strength
are greater than the one of coir fiber coming from other countries.
Table 4.4 Mechanical properties of treated and untreated coir fibers
Tensile Elongation
Diameter Reference
Properties strength of break
[µm]
[MPa] [%]
Coir untreated 211.7 51.13 100-149

Coir treated 267.7 62.55 100-149
Indonesia coir 218.25 46.02 - [Bakri, 2010]

Brazil coir 75.0 29.5 - [Silva et al. 2000]
Indian coir 175.6 34.0 - [Kulkarni et al. 1981]
Tanzania 68.4 21.2 - [Ezekiela et al., 2011]
95
The conclusion shows that the treatment of coir fibers increases the
tensile strength and delivers higher value to the elongation of a break than
the ones of untreated fibers. Average tensile strength of treated fiber is as
twice greater than the one of untreated. Based on these results, coir fiber
after treatment presents an improved ductile. Indonesian coir fiber has
ductile properties suitable for use as reinforcement in concrete composites
with high ductility.
The treatment significantly removes impurities on the fiber surface,

resulting in surface modification and improved thermal stability. TGA
measurements revealed that the treatment of fibers has a positive impact
on the thermal stability of the sample.
SEM observation shows that water treatment has a significant

impact of on the surface of the fibers (removing impurities, decreasing the
siliceous compounds content) and decreases the average diameter of the
fibers. These changes in fiber structure induce an improvement of the
macroscopic behavior of the fibers.
96
CHAPTER.5.
DESIGN, RHEOLOGY PROPERTIES,
MICROSTRUCTURE, AND RHEOLOGY MODEL OF
PRODUCT EXTRUDED FIBER COMPOSITES
5.1. Introduction
This study aims to obtain extruded building materials with low

environmental impact. Mortar/cementitious is the basic ingredient of concrete
used in this study that is made with cement, sand and clay. The mortar based
materials are reinforced with natural fibers of coconut plants. The use of natural
fibers and clay as raw materials are readily available locally at every place in the
world. They are sustainable raw material for local construction, and their use
reduces transportation, economic costs, and environmental impact.
The tested mix design is a development of the results already obtained.

This study is conducted to evaluate the rheology of the coir fiber reinforced
cementitious composites (CFRCC). In this section, the effects on the rheology of
fiber content, fibers length and percentage of cement are studied. The cement-
based materials extrusion technology to set up that is necessary to perform an
adequate rheological characterization of the cement-based formulations. The
rheological characterization is fundamental for the development of a new extruded
product if we take into consideration some basic aspects (mix composition,
cost/performances ratio, process parameters).
The process of designing a mixture of cement, sand and clay was studied
for different contents of cement. The first study deals with the influence of
water/cement ratio in mortar mix to ensure an extruder flow providing hardened
extrudates without defects. Rheological properties of the materials were studied.
According to Toutou et al. work, extrudability criterion is that the yield stress
value should be at least equal to 20 kPa. [Toutou, 2005]. Moreover, mixture
extrusion flow needs to be stabilized during processing; local drainage may cause
surface defects. A avoid such defects, homogeneous nature of the material during
extrusion should still be maintained [Perrot, 2007]. A prediction of the yield stress
of coir fiber-reinforced cementitious composite is also proposed, develop the
model provided by Ferec et al. [Ferec, 2014].
97
The final result obtained in this study is the formulation of an extrudate
composite taking into accounts the effects of fiber content on the material
rheology. After the examination of the fresh concrete is continued in the following
chapters an examination of the hard mortar on the chapter 6. The design of
composite material used to study the performance of mechanics of materials.
5.2. Mix-Design of low cement content in mortar for extrusion
The formulation of an extrudate paste is performed using a rheometer. The

designed cement-based paste should be hard enough to hold its shape once
extruded and soft enough to flow inside the extruder. Materials are having a yield
stress of 20 kPa meet these conditions [Toutou et al., 2005]. The vane test was
used to evaluate this rheological property of the mortar samples. It was carried out
using a speed-controlled rheometer equipped with a four-bladed vane, measuring
8.8 mm in width and 10 mm in length. Rotation speed is controlled, and the torque
is measured.
The effect of water content on the yield stress of fresh mortar containing
various amounts of kaolin and cement is therefore studied to find the optimized
mix design for fresh material dedicated to extrusion.
5.2.1. Mix design of an extrudable mortar.
The product development consists in investigating the feasibility of using

extrusion technology to fabricate construction products. The best material
water/cement ratio must be found to meet criteria of extrudability. If poor shape
stability phase migration, excessively high extrusion pressure, or surface defects
(usually edge tearing) were observed, the material was considered as not
extrudable.
This mix design approach for each studied mixture leads to the sample
extrudability. Mixes are tested with superplasticizer/High Range water Reducing
Admixture (HRWRA) to reduce the water content and increase mechanical
strength [Khelifi, 2013]. The superplasticizer content is1.5% by weight of cement.
Different cement to clay/kaolin ratio was tested. The mass proportion of sand is
60%. For extrudate material, the ratios of cement and clay used were at maximum
40%. The material compositions of eight mix designs for the project are
summarized in Table 5.1.
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Table.5.1. Mixture proportions of cement, clay, and sand
Mixture name Cement (%) Clay (%) Sand (%)
K40S60 0 40 60
C5K35S60 5 35 60
C10K40S60 10 30 60
C15K25S60 15 25 60
C20K20S60 20 20 60
C25K15S60 25 15 60
C30K10S60 30 10 60
C40S60 40 0 60
Gradually the water was added to achieve a yield stress approaching 20

kPa. The relationship between water content ensuring such yield stress with
cement content is an exponential function as shown in Figure 5.1, with the
following formula:
W/C = α e - βC …..…………………….……… (5.1)
Where: W/C is the water/cement mass ratio in percentage, C is the cement content
in percentage and α, β is coefisien regretion parametre. For this composition α =
21.532; β = 0.015.
For the composition made with 40% of cement and 60% of sand
(C40S60), the amount of water content by weight of cement is W = 0.12. While
the composition of 40% of Kaolin and 60% of Sand (K40S60) is the amount of
water content by weight cement is W = 0.22. The water content in the clay mortar
is almost twice the water contained in the cement mortar. We note that a mixture
of 40% cement and 60% clay exhibiting a yield stress of 20 kPa produces a very
stiff paste that does not flow under its weight.
Figure.5.1. Water content vs. cement content in mortar for a yield stress of
20 kPa
99
5.2.2. The water content in clay mortar.
In this part, we study how the torque varies with water content. The mass
composition of the mortar mix is made with 40% of kaolin clay and 60% of sand
(K40S60). Vane test results showed that the value of the torque increases while
some water decreases. Also, the time to achieve the maximum of torque increases
when the water content decreases (Figure 5.2).
Figure. 5.2. The torque vs. time curves for clay mortar (K40S60) containing
different masses of water
Rheological properties of the clay mortar (K40S60) showed that

increasing water cement on clay will decrease the yield stress (Figure 5.3) and that
the following exponential empirical relationship can describe accurately this link
(R² = 0.9982):
𝜏 = α e - βW ……………………………..…………………………..(5.2)
where 𝜏 is the yield stress (kPa) ; W = Water (%); for K40S60 α = 324.8;
β=0.119
100
Figure. 5.3. The yield stresses vs. water content in clay mortar
5.2.3. Influence water content on cement mortar.
The water content of an extrudible mortar made of 40% cement and 60%
sand (C40S60) in mass is searched. A yield stress of 20 kPa is found for a water
content of 0.12 as shown in Figure 5.1. The surface aspect of the sample is not
smooth. Also, the sample surface presents crack lines. Such aspect does not match
extruded criterion on surface texture
Conditions of extruded material with a smooth surface without defects are

obtained with the addition of water/cement gradually. According to rheometer
tests (section 3.4.4.), a smooth surface for the composition C40S60 is obtained at
water content/cement of 0.14. At this water content, the torque measured during
the vane test is 20 Nm. Then, using the formula Eq. (3.5) the computed yield
stress is 12 kPa.
Similarly to kaolin mortar, vane test results showed that the value of the
torque increases while some water decreases. Also, the time to achieve the
maximum of torque increases when the water content decreases (Figure 5.4).
101
Figure. 5.4. The torque vs. time curves for cement mortars containing
different amount of water
Rheological properties of the cement mortar (C40S60) showed that

increasing water cement on clay will decrease the yield stress (Figure 5.5) and that
the following exponential empirical relationship can describe accurately this link
(R² = 0.9875):
𝜏 = α e -β W ………………………………………… (5.3)
Where, 𝜏 is the yield stress (kPa), W is the water content in percentage and for
C40S60 α = 1238.4 ; β=0.331
Figure. 5.5. The yield stresses vs. water content in cement mortar
102
5.2.4. The formulation of an extruded fiber reinforced composites.
Low cement content and use of local natural materials are common ways
to design an environmentally friendly material. For this reason, the following two
compositions (called C1 and C2) are chosen: C10K30S60 made with 10% of
cement content and C20K20S60 made with 20% of cement. The yield stress of
about 20 kPa was obtained for an amount of water of 0.18 by weight of cement
(Figure 5.6). While C2 required a water content of 0.16 by weight of the cement
to reach the targeted yield stress (Figure 5.7).
The formulation of the fiber-reinforced mortar composites consists in

finding the required water content needed to achieve a 20 kPa yield stress needed
for an optimized extrusion. The water content is then kept constant even for
composites containing up to 5% of fibers volume content.
Figure. 5.6. Torque versus time curves obtained during vane tests mix-design
C1 (yield stress of 20kPa)
C2 (yield stress of 20kPa)
103
During rheological vane tests measurements, torque is the important parameter
recorded to compute the properties of cement mortars. This parameter is linearly
linked to the material yield stress. For mix-design C1, a water content of 0.21
leads to a maximum recorded torque of 20 µNm (Figure 5.8). Such torque leads to
a 13 kPa yield stress that is found to be sufficiently high to ensure stable extruded
samples exhibiting surface without defect (Figure 5.9.).
type C1
Figure. 5.9. Surface of the extruded mortar type C1
For the mix-design C2, the same observation is made. A water content of
0.19 which leads to a yield stress of 13 kPa (20 µNm see figure 5.10) can provide
extrudates which sustains gravity and presents a smooth surface without defect.
104
Figure. 5.10. Torque versus time curves obtained during vane tests mix-
design type C2.
Figure. 5.11. Surface of the extruded mortar type C2
Figures 5.9 and 5.11 suggest that a yield stress of 13 kPa (maximum torque of
20 µNm) is enough to ensure that the extrudate can sustain gravity after extrusion.
Therefore, a maximum torque of 20 µNm is targeted for the mix design
procedure.
The figure showing the relationship between water content ensuring a
maximum torque of 20 µNm and the cement content is plotted in Figure 5.12.
The cement content is linearly decreased when the amount of water content
increases. Empirical formula R² = 0.9847is able to describe this linear link:
W /C = α - β*C ……………………………………………….. (5.4)
Where: W is the water content in percentage, C is the cement in percentage, α =

24.842 ; β=0.294
Figure 5.13 shows the surface aspect of extruded mortar for a paste exhibiting a
yield stress of 13 kPa. We can see that the extrudate surface is smooth.
105
Figure. 5.12. Water content and cement content in mortar for Torque 20 µNm
.
Figure. 5.13. Surface of the extruded cement mortar
Table 5.2. Mix formulation of the coir fiber-reinforced fresh cement mortar
for extrusion.
Composite Cement Clay Sand SP Water Fiber Fiber Fiber
name (%) (%) (%) (%) (%) 5mm 10mm 15mm
(%) (%) (%)
C1-0 10 30 60 1.5 21 0
C1-2-05 10 30 60 1.5 21 2
C1-3-05 10 30 60 1.5 21 3
C1-4-05 10 30 60 1.5 21 4
C1-5-05 10 30 60 1.5 21 5
C1-2-10 10 30 60 1.5 21 2
C1-3-10 10 30 60 1.5 21 3
C1-4-10 10 30 60 1.5 21 4
C1-5-10 10 30 60 1.5 21 5
C1-2-15 10 30 60 1.5 21 2
C1-3-15 10 30 60 1.5 21 3
C1-4-15 10 30 60 1.5 21 4
C1-5-15 10 30 60 1.5 21 5
106
C2-0 20 20 60 1.5 19 0
C2-2-05 20 20 60 1.5 19 2
C2-3-05 20 20 60 1.5 19 3
C2-4-05 20 20 60 1.5 19 4
C2-5-05 20 20 60 1.5 19 5
C2-2-10 20 20 60 1.5 19 2
C2-3-10 20 20 60 1.5 19 3
C2-4-10 20 20 60 1.5 19 4
C2-5-10 20 20 60 1.5 19 5
C2-2-15 20 20 60 1.5 19 2
C2-3-15 20 20 60 1.5 19 3
C2-4-15 20 20 60 1.5 19 4
C2-5-15 20 20 60 1.5 19 5
All the ingredients are expressed as weight proportion of cement content.
Finally obtained mix designs of low cement content materials are listed in
Table 5.2. Composite materials under conditions of constant water/cement content
with fibers added to the mix will be then tested. Furthermore, the yield stress of
fiber reinforced paste will be measured using the vane test. Compositions C1 and
C2 are used to make composites reinforced with fibers. For both Composites, the
water/cement (w/c) ratios are 0.21 for C1 and 0.19 for C2. Fibers lengths of 5, 10
and 15 mm; and, fiber contents of 2%, 3%, 4% and 5% (by weight of cement)
have been used.
5.3. Morphologies of fresh fiber mortar composite
Analysis of the morphologies of the mortars is performed using optical

microscopy. Mortars are first cured for 28 days. Samples were observed after the
process of mixing and after extrusion.
Figure 5.14 shows the composite mortar after mixing with a mixer. Fiber
placement does not seem to be randomly and well dispersed. Furthermore, to
obtain a more compact material with fibers dispersion and forming needs to be
performed by screw extrusion.
Observation of the microstructure after the mixer and cured for the fiber
concentration of 2% by weight of cement is shown in Figure 5.15, the distribution
of fibers in the matrix seems random. The matrix with the fiber concentration of
4% by weight of cement is also shown in Figure.5.17. Another case of fiber
concentration of 3% by weight of cement can be also seen in Figure.5.16A with
problems of fibers entanglement. However, after further examination, we can see
107
that each fiber stands alone and can be easily dispersed. As well there are holes or
pores as shown in Figure.5.16B. It can be homogeneous after mortar formulations
through the process of molding and extrusion processes.
Figure. 5.14. Morphology of fiber-reinforced cementitious composites after

mixing.
Figure. 5.15. Morphology of fiber-reinforced cementitious composites, fiber

content 2%

content 3%
108
content 4%
Holes or pores are still visible, either in mortar formulations with low fiber
content and high fiber content as shown in Figure.5.15; Figure.5.16 and
Figure.5.17. Also, Interfacial microstructure of the fiber and matrix in fresh
showed scattered randomly. The fiber out of the matrix indicates wrong position.
That means a good adhesion between the fiber and the matrix (Figure.5.18).
Similarly, the fibers are embedded in a matrix showing the presence of bonding
between the fiber and the matrix (Figure.5.19). Hence, the mortar will become
solid after going through the process of compaction in a mold or by screw
extrusion.
Figure. 5.18. Microstructure adhesion of fiber out of matrix
109
Figure. 5.19. Microstructure adhesion of fiber embedded in a matrix
5.4. Rheology properties of fiber mortar composite

extrudability
The knowledge and understanding of material extrusion allow rheology to

be used for quality control and product development. There is a need for quality
control testing through rheology. It is feasible to use the current rheometer to
evaluate the rheological behavior of Coir Fibers reinforced mortar composites. It
is important to note that for firm paste extrusion, the yield stress is the most
relevant parameter that could be used for quality extrusion control. Viscous
effects remain limited due to the reliability low shear rates used in firm pastes
extrusion.
The flow properties of the fresh material are a key point as fibers can
move and to orient due to the concrete flow. Therefore, fibers may induce
anisotropic and heterogeneous mechanical behavior that depends strongly on their
dispersion and orientation state [Ferrara et al., 2011], [Kang et al., 2011], [Kuder
et al., 2010], [Sanal et al., 2013]. It is well established that fiber orientation
depends on both process and material rheology [Boulekbache et al., 2010],
[Ozyurt et al., 2007], [Kuder et al., 2010], [Martinie et al., 2011], [Perrot et al.,
2013]. The previously cited works highlight the yield stress of fiber reinforced
concrete is a key parameter controlling and limiting the fibers orientation under
flow. Then, some works have been carried out on the effect of fibers on the
concrete rheology, [Kuder et al., 2007], [Martinie et al., 2010], [Ghanbari et al.,
2009], [Kaufmann et al., 2006], [Li and Li, 2013] and on the prediction of fiber
orientation during processing [Martinie et al., 2013], [Laranjeira et al., 2012]
[Ferec, 2015].
Published literature on the correlation between cementitious composite
rheological properties and fiber volume or dispersion has typically focused on
110
rigid steel fibers. It has been shown that increasing fiber volume fraction and
aspect ratio decreases the workability of cementitious composite materials
[Dhonde 2007], [Martinie 2010]. However, there has been no publication using
natural fiber /coir fiber for cement mortar composites.
5.4.1. Fiber content and fibers length on torque
The used coir fibers i are almost produced through a process of washing
and drying. Such results are obtained in the previous chapter, the used diameter
ranges between 50 and 200 µm with a density of 0.86 g / cm3.
The torques recorded during vane test measurements for fresh fiber-
reinforced mortar composites with different water, and fiber contents are shown in
Figure 5.20 for fibers length of 5 mm, Figure 5.21 for 10 mm and Figure 5.22 for
15 mm. It can be seen that torques of all composites increase with fiber content. It
is consistent with the phenomena described in a recent study [Martinie 2011]
[Ferec 2015] [Feng 2013].
Figure. 5.20. Torque vs. time for different fiber contents - fibers length of
5mm. (a) C1 and ( b) C2
111
Figure.5.21.Torque vs. time for various fiber contents - fibers length of
10mm. (a) C1 and (b) C2
Figure.5.22.Torque vs. time for different fiber contents - fibers length of

15mm. (a) C1 and (b) C2
5.4.2. Fibers content and fibers length on yield stress.
The yield stress increases with fiber content and fibers length. The yield
stress is plotted against the fiber content, fibers length for both types of the matrix
(C1 and C2) as shown in Figure. 5.23 For fibers length of 5 mm, in Figure. 5.24
For fibers length of 10 mm and in Figure. 5.25 For fibers length of 15 mm. In
general, the yield stress increases as the fiber content, and fibers length increase.
This phenomenon is expected because water–solid mixture with higher water
content should require a smaller shear stress to flow. In general, the yield stress
for the mix-design type with a cement content of 20% (C2) is greater than the one
measured with mixtures containing 10% of cement (C1). In other words, more
clay content gives a lower yield stress value.
The combined effects of the fiber content and fibers length has been
studied by fitting empirical relationships on experimental data fibers length. The
best fitting curves with their equation and correlation coefficient R2 value are
112
summarized in Table 5.3. The yield stress formulation is based on tests carried out
for matrix C1, C2 and fibers length of 5 mm, 10 mm and15 mm with fiber
contents of 2%, 3%, 4% and5%. The used empirical relationship can be written
as follow:
……….…………… (5.5)
where: Fc is the fiber content (%); yc is the yield stress (kPa); , are fitting
parameters.
Table.5.3. Fitting parameters values for the tested materials

Fiber Parameter
Correlation Parameter
Mixture name length
coefficient
(mm)
5 0.9669 11.710 0.0928
C10K30S60 10 0.9967 11.983 0.1042
( C1 ) 15 0.9680 12.593 0.1094
5 0.9622 12.314 0.0870

C20K20S60 10 0.9991 12.733 0.1034
( C2 ) 15 0.9545 13.328 0.1073
Figure. 5.23. Yield stress vs. fibers contents for fibers length of 5mm
113
The best-fit curve obtained and its equation (5.6) and R2 value are
presented in the graph for easy reading. A relatively good r2 value of 0.99 has
been achieved, indicating that the yield stress is dependent mainly on the fiber
content. Nevertheless, it still appear that the yield stress is dependent not only on
the fiber content but also on the fibers length.
Figures 15.26 and 15.27 show the effect of increasing the fiber content of
yield stress for different fibers length (5mm, 10mm and 15 mm), respectively for
matrix C1and for matrix C2. These figures show the effect on the yield stress of
different fibers length. It is clear that both yield stress increase with increasing
fiber content and fiber length and decreasing water/cement ratio.
114
Figure. 5.26. Relationship between the yield stress and fibers content for C1
Figure. 5.27. Relationship between the yield stress and fibers content for C2
5.5. Rheology model
In Section 5.4, the existence of a meaningful relationship between the

yield stress and the fiber content has been evidenced. In the case of properties of
fresh cementitious materials, it has been shown that addition of fibers decreases
the workability of the material. This effect increased with fibers volume fraction.
To predict the yield stress of fiber-reinforced cementitious composites dedicated
to extrusion, a physical modeling can be searched. The mortar yield stress
depends on a relative yield stress that depends on the aggregate volume fraction,
115
fiber aspect ratio (ratio of the fibers length over the average fibers diameter) and
fiber volume fraction.
Martinie et al. provide a classification of the fiber stiffness according to

the ratio of concrete yield stress over elastic fiber strain. They also show that steel
fibers can be considered as rigid if the deformation of the fibers due to shearing
remains negligible in front of the fibers length. It is shown that the rheology
model initially developed for spherical inclusions and aggregates can be adapted
to fibers [Mahaut et al. 2008], [Martinie et al. 2010], [Perrot et 2013]. Férec et al.
have developed a prediction model of the yield stress. For suspensions of steel
fibers dispersed in kaolin paste, (a non-Newtonian fluid exhibiting a yield stress)
by taking into account hydrodynamic and fiber interactions [Férec et al., 2014].
However, existing studies focus on rigid fibers, while no study has attempted to
model the yield stress of suspension containing flexible fibers such as natural ones
The objective of this study is to propose a model containing adjustable

parameters that are determined by fitting experimental data of yield stress values
for freshly-made coir fiber-reinforced mortar composites. In a first attempt, the
model developed by Ferec et al. is tested.
5.5.1. Relative yield stress as a function of the fiber factor
In this section, we focus on the relationship between the yield stress and
the fiber factor (r øf). The fiber factor is a multiplication between the fiber
volume fraction (øf) with the fiber aspect ratio (r). The fiber aspect ratio (r) is a
ratio of the fiber length (Lf) over the fiber diameter (Df ). Relative yield stress can
be plotted as a function of the fiber factor as shown in Figure 5.28 for type mix-
design C1 and Figure 5.29 for mix-design C2. The background of the yield stress
prediction model used here was developed from the model developed by Ferec et
al., 2014 and then compared with experimental results. The presence of fiber
induces an anisotropic yield stress depending on how the fiber orientation. Under
a critical shear rate, the tendency of the fibers to get oriented in the flow direction
is overcome by the particle-particle interactions. At higher shear rates, the
hydrodynamic interactions become more important, and the fibers get oriented.
The shear yield stress value for an isotropic fiber orientation state of the
composite can be written as follow:
………………………… (5.6)
………………………..(5.7)
116
Where, is a component of the isotropic orientation tensor.
The predicted relative yield stress for an isotropic fiber orientation state can obtain
from Eq. (5.6) Moreover, Eq. (5.7) Moreover, written as Eq. (5.8):
………………………… (5.8)
The relative yield stress ( ) is the ratio between the yield stress of the paste
containing fibers and the yield stress of the kaolin paste without any fibers.
With the addition of the rigid fibers, the relative yield stress increases with a
significant enhancement at fiber factor close to 3.5. The values of the fiber factor,
when this critical concentration is reached cited in the literature are between 0.2
and 2 depends on the other components in the materials tested [Banfill et al.,
2006].
The results obtained with the addition of natural fiber show that the
relative yield stress increases with a significant enhancement of fiber factor close
to 14 for type mix-design C1 as illustrated in figure 5.28. For mix-design C2, r the
relative yield stress increases with a significant enhancement of fiber factor close
to 15 as shown in figure 5.29. The identification of the parameters is given in
Table 5.4.
For fiber sizes of 5 mm and 10 mm, the model gives excellent results in
agreement with the experimental data. However, it does not apply to a larger size
(15mm). This result is the same as that produced by Ferec et al., 2014, some
discrepancies observed for suspensions with fibers having an aspect ratio of larger
than 30.
Table.5.4. Parameter value of the yield stress model
Fiber length Parameter

Mixture name
(mm) (kPa)
5 2.20
C10K30S60 ( C1 ) 10 0.74
15 0.40
5 1.59
C20K20S60 ( C2 ) 10 0.95
15 0.55
117
Figure. 5.28. Relative yield stress as a function of the fiber factor
for the model predictions type C1.

for the model predictions type C2.
118
5.5.2. The proposed rheological model to predict yield stress
The Ferec et al. model does not provide accurate results for the longest
size. To improve the prediction ability of the model, we try to adapt the Ferec
model empirically to make it suitable for all the tested fiber lengths.
Figure 5.30 dan Figure 5.31 show the experimental results along with the
adapted Ferec model. We add a linear term to the Ferec model to best fit our
experimental data. The Prediction model now writes:
……………….. (5.9)
Fitted curves show an excellent agreement with experimental data. The value of
the identified parameters is given in Table 5.5 where, the value of the parameter R
decreases with the fiber aspect ratio. In contrast to the S parameter, this increases
with the fiber aspect ratio.
Table.5.5. Parameter value of modification the yield stress model

Fiber length Parameter Parameter
Mixture name
(mm) (kPa) (kPa)
5 1.8 1.55
C10K30S60 10 0.45 1.65
( C1 )
15 0.19 1.75
5 1.4 1.5
C20K20S60 10 0.35 1.7
( C2 )
15 0.145 1.8
119
for modification the model predictions type C1.

for modification the model predictions type C2.
120
5.5.3. Validation the rheological model.
The experimental results validate the prediction model as shown in Figure

5.32 for mix-design C1 and Figure 5.33 for mix-design C2. It is also interesting to
sum up data from all experiments (C1 + C2) as shown in Figure 5.34. Table 5.6
provides parameters value of modification the yield stress model versus
experimental data.
………………….. (5.10)
Table.5.6. Parameter value of modification the yield stress model

Correlation Parameter Parameter
Mixture name
coefficient A B
C1 0.9992 0.9982 0.0042
C2 0.9987 01.0017 0.0009
C1+C2 0.9914 0.9844 0.0361
Figure. 5.32. Model versus experimental yield stresses for type C1.
121
Figure. 5.33. Model versus experimental yield stresses for type C2
Figure. 5.34. Model versus experimental yield stresses for type C2
This present work shows that the yield stress model used for common
mortar can be generalized to fiber reinforced concretes. Indeed, it predicts the
evolution of the yield stress of the fiber-reinforced cementitious composite.
122
Rheological behaviors of cement mortar and fiber reinforced cementitious
composite are presented in this chapter. The formation of clay material through
extrusion produces a compact material with the surface without defects.
The rheological approach serves as an effective plain cement mortar fresh

property design guide for achieving hardening properties of the fiber cement
mortar composite. The rheology is important for the characteristic of fresh cement
paste, grout, and mortar and concrete to perform in practical applications. It is
used for the desirable properties of the hardened materials can be achieved.
The formulation of a material with low cement and from local materials
that can be extruded with smooth and compact aspect has been studied. As
expected, Clay absorbs more water than cement. Therefore, the amount of clay
and water - cement will influence the extrusion results.
Mix design of mortar obtained from cement, clay and sand in the ratio of
the weight of 10:30:60 respectively requires 18 % water - cement. As for the
proportion of water - cement 20:20:60 needs a 16 % to produce the extruded
material. The addition of fibers into extruded formulations requires the addition of
water to obtain an extrudate mortar. To counter the loss of workability due to the
addition of the selected fiber mortar mixture basic (plain mortar) without adding
extra water. Furthermore, taking into account the addition of fibers up to 5 % by
weight of cement, to remain in the extruded condition, for 10 % of cement
formulations need a water - cement ratio of 21 %. As for the 20 % cement
formulations needed water - cement ratio of 19 %.
The yield stress increases with fiber content and fibers length. The more
clay content gives a lower yield stress value. Rheology models for coir fiber
reinforced cementitious composites have been obtained. The model of prediction
yield stress:
The model prediction shows a good agreement with the yield stress values of coir
fibers reinforced cementitious composites.
The observations of the surface of the fiber cement mortar composites
before extrusion are seen the small holes/ microporosity between the mortar
matrix. Also, the visible concentration of fibers in the mix has not spread. That
required the formation of materials using extrusion to the more evenly spread of
fibers.
123
CHAPTER.6.
MECHANICAL PERFORMANCE,
MICROSTRUCTURE, FAILURE MODE, AND MODEL
OF SCREW EXTRUDED FIBER COMPOSITES USING
DESTRUCTIVE TESTING METHOD
6.1. Introduction
Recently, interest in the composite in construction material has shifted
towards the use of natural fibers as a reinforcement component because potential
environmental benefits. The advantages of natural plant fibers, such as low
abrasion, multi-functionality, low density, low cost, ready availability and relative
ease of waste disposal, encourage their application in composite materials.
Almost all of the commonly available natural plant fibers that are cheap and
abundant in nature. There are being used for reinforcement in combination with
non-biodegradable matrix materials such as unsaturated polyester, epoxy resin,
polyethylene, polypropylene and cementitious. Natural fibers have been
successful in imparting to composite materials certain benefits like reduced
machine wear compared with synthetic reinforcement materials and a lowering of
associated health hazards.
The mechanical properties of natural cellulosic fibers are a function of

several variables, the most important being the spiral angle and the cellulose
content. The superior flexibility of natural fibers, when compared with that of
glass fibers, enables them to bend rather than fracture during processing. The
compressive parameter strength and tensile strength are very often used to
quantify the quality of cementitious materials. Mechanical performance fiber
reinforced cementitious represent a new generation of construction materials for
the 21st century now being actively researched [Andiç-Çakir et al., 2014], [Ali M
et al., 2012]. Fiber additions offer a convenient and practical means of achieving
improvements in many of the mechanical properties of cement, mortar and
concrete such as enhanced compressive strength and tensile strength.
In the present work, fiber composites are developed, and their mechanical
properties are evaluated. The fibers used in the study included coir fiber. Cement
mortar was used as the matrix. In this context, the compressive strength measured
at 28 days after casting. The compressive and tensile characteristics of extruded
124
coir fiber reinfoced cementitious composites (CFRCC) were determined by
testing a minimum of three-four cylinder specimens for each batch using the
Mechanical Testing System (MTS) Instron 8803.
This investigation was carried out to evaluate the results of the mechanical
performance of CFRCC under static loading. CFRCC in the present investigation
is tested using screw extrusion for compressive and splitting tensile strength
behavior. Stress-strain under compressive and tensile load was studied to provide
insight into the behavior and failure mechanism of CFRCC composite. Effect of
fiber content and fiber length evaluated to mechanical performance. To analyze
the mode of failure for compression, tensile, several optical photographs were
taken to study the mechanism distribution of coir fiber in cement mortar.
6.2. The aspect surface of screw extrusion.
Aspects surface of the screw extrusion process is observed. It is the

relationship with the rheological results in designing composite materials.
Observations were made on mortar extrusion, composite extrusion and comparing
the results with the outcome of the extrusion mold.
6.2.1. Surface of extruded mortar
The results surface observations of cement mortar are shown in Figure 6.1
the surface aspects of cement mortar for 10% cement (type C1) and 20% of
cement (type C2). As well as shown on the Figure 6.2 surface aspect on a cross
section of the cement mortar showed results a smooth flat surface. It shows that
the presence of sufficient amount of water necessary so that the material extruded
material well, mentioned extrudability.
Figure. 6.1. Aspect surface cement mortar extrudability: (a) type C1, (b)
type C2
125
Figure. 6.2 Aspect surface of cross-section of cement mortar extrudability:
(a) type C1 and (b) type C2
6.2.2. Surface of extruded composites
The extrusion results are shown in Figure 6.3 for aspect surface of
CFRCC, the type C2 of 20% cement mix: (a) 2% fiber, (b) 3% fiber, (c) 4% fiber.
While, the results is shown in Figure 6.4 for aspect surface of CFRCC composite
type C1 of 10% cement mix: (a) 2% fiber, (b) 3% fiber, (c) 4% fiber. The both
give the same result aspect surface, namely flat and smooth. It shows that the
materials are extrudability.
(a) (b ) (c)
Figure. 6.3 Aspect surface of coir fiber cement clay mortar composites
extrudability type C2: (a) 2% fiber, (b) 3% fiber, (c) 4% fiber.
(a) (b) (c)
Figure. 6.4 Aspect surface of coir fiber cement clay mortar composites
extrudability type C1: (a) 2% fiber, (b) 3% fiber, (c) 4% fiber.
126
6.2.3. Surface of mold and extrusion
The results obtained of the mold in comparison with the extrusion process
as shown in Figure 6.5.The aspect surface of CFRCC composite forming using:
(a) Mould and (b) Extrusion.
Although the process of formation of the test material to the mold through
compaction ten layers, then compacted with ten knocks then through vibration and
removed after 24 hours. The results obtained are uneven, not smooth surface
defects as well as the extrusion process.
Figure. 6.5 Aspect surface of coir fiber reinforced cementitious composites

forming using: (a) Mould and (b) Extrusion
6.3. Orientation fibers in screw extrusion.
This orientation can have significant consequences on the mechanical

properties when cured, positive or negative depending on the compatibility of
fiber orientation directions with solicitations. Several studies have shown the
influence of fiber orientation on the behavior of material [Shah et al., 1994; Shao
et al., 1997]. In the case of forming by extrusion, the fibers undergo an orientation
induced by the process. The process, under the effect of shear in the shaping zone,
The fibers oriented preferentially in the direction of the extrusion flow [Mobasher
et al., 1998] [Akkaya et al., 2000]. Most of the time, fibers are oriented in the
longitudinal direction. The ductility compared to those with fibers having random
orientation [Absi et al., 1994] [Swamy et al., 1975].
The results of the observations under an optical microscope of fiber

composite after going through the process extrusion after 28 days, showing the
hole diminished and deployment of fiber evenly. As the visible fibers at random
positions, there is a longitudinal direction and the transverse orientation of the
127
direction extrusion as shown in Figure 6.7 for longitudinal direction and Figure
6.8. for direction transversal. Cutting the fiber direction is longitudinal (L), and
transverse (T) after extrusion is shown in Figure 6.6.
Figure. 6.6 Direction of extrusion of fiber reinforced cementitious composites,

Longitudinal (L) and Transversal (T).
6.3.1. Longitudinal
In observation of the composite material obtained fiber direction

lengthwise direction is random. The deeper observations, shown in Figure 6.7
there is a fiber cut in the transverse direction, and the fibers are embedded
lengthwise.
Figure. 6.7 Morphology fiber cement mortar composites after extrusion, the
longitudinal direction of extrusion (L).
128
6.3.2. Transversal
Similarly, the observation of the composite material obtained in the transverse

direction toward the fiber is scrambling. Deeper observations, shown in Figure 6.8 as well
as on pieces lengthwise, fibers are severed in the transverse direction, and the fibers
embedded lengthwise.
Figure. 6.8 Morphology fiber cement mortar composites after extrusion, the
transversal direction of extrusion (T).
6.4. Mechanical performance extruded composites.
The performance of mechanics of CFRCC materials observed in the

compressive stress-strain, the tensile stress-strain, and the extrusion process
compared to the molding process. The experimental observations are results of
stress and strain relationships.
6.4.1. Compressive stress-strain of extruded composite
Figure 6.9 shows the experimental results of the stress-strain

characteristics of extruded CFRCC in typical compressive stress-strain curves of
mortar and composite with a fiber length of 5 mm. The result shows that average
the peak stress in the compressive strength values of wash-dry treated coir
composite was 23% higher than that of the cement mortar (control sample).
Compared Andiç-Çakir et al. (2014) increase in the compressive strength

values were 3.64% of the control sample for untreated coir incorporating ones and
129
9.00% of the control sample for alkali treated coir fiber incorporating mortars.
Compared with untreated and treated an increase in compressive strength of one
and a half time.
Improved performance with a compressive strength of 5 mm fiber length

in the same fiber content 4% is an increasing one and a half time in the
compressive strength of CFRCC materials in extrusion only with treatment by
washing and drying.
Figure. 6.9.Typical compressive stress-strain curves mortar and composite

with fiber length of 5 mm for extruded samples
Figure 6.10 shows the experimental results of the stress-strain

mortar and composite with length fiber 10 mm of under forming using extrusion.
It found that the peak stress of CFRCC was 30% higher than that of cement
mortar. The result of the compressive strength increase of 2.3 times compared the
result of Andiç-Çakir et al. (2014).
Figure. 6.10. Typical compressive stress-strain curves mortar and composite

130
Figure 6.11 shows the experimental test results of the stress-strain
mortar and composite with length fiber 15 mm of under forming using extrusion.
It found that the peak stress of CFRCC was 37% higher than that of cement
mortar. The result of the compressive strength increase of three times compared
the result of Andiç-Çakir et al. (2014).
Figure. 6.11. Typical compressive stress-strain curves mortar and composite

23% increased the compressive stress of CFRCC for 5mm, 30% for 10mm
and 37% for 15mm fiber length, compared to cement mortar. The results obtained
with the addition of fiber increased compressive stress with increasing fiber
length. That is due fiber retain cracking, thus improving the behavior of materials.
Compared with the results Andiç-Cakir et al. (2014) without extrusion obtained
there were increased compressive stress 1.5 times of 5 mm fiber length, 2.3 times
of 10 mm fiber length and 3.0 times of 15 mm fiber length for extrusion materials.
The compressive stress of the CFRCC have shown a gradual increase by

increasing fiber length, and these values are higher for treated fibers when
compared to untreated ones. Likewise, the extruded material provides increased
compressive stress compared to the manual process.
6.4.2. Tensile stress-strain of extruded composite
Several studies have shown that the splitting tensile test is simple and
reliable, giving reasonable results on resistance to direct traction compared to the
bending test. Tensile strength was observed until cracks in the mortar characterize
the mortar strength.
Figure 6.12 is the experimental test results of typical tensile stress-strain

curves cement mortar and fiber composite with length fiber 5 mm of under
131
forming using extrusion. It found that the peak stress of CFRCC was 29% higher
than that of cement mortar.
Figure. 6.12.Typical tensile stress-strain curves mortar and composite with

length fiber 5 mm of under forming using extrusion
Figure 6.13 is the experimental test results of the stress-strain

characteristics of extruded CFRCC and cement mortar with length fiber 10 mm of
under forming using extrusion. The peak stress of CFRCC was 30% higher than
that of cement mortar.

length fiber 10 mm of under forming using extrusion.
Figure 6.14 is the experimental test results of typical tensile stress-strain

curves cement mortar and fiber composite with length fiber 15 mm of under
forming using extrusion. It found that the peak stress of CFRCC was 41% higher
than that of cement mortar.
132
length fiber 15 mm of under forming using extrusion.
29% increased the tensile stress of CFRCC for 5mm, 30% for 10mm and
41% for 15mm fiber length, compared to cement mortar. The results showed that
the performance CFRCC tensile stress increases with increasing fiber length
compared to cement mortar. The increase of tensile stress is higher than the
increase compressive stress.
6.4.3. Stress-strain of molded and extruded sample behavior
The evolution of compressive stress of cement mortar manually processed

through the molding and extrusion process is shown in Figure 6.15. In the Figure also
shows a comparison between the compressive stress of the 10% cement content of type
C1 and 20% cement content of type C2. The results showed that performance
compressive stress can be improved through the extrusion process when compared to the
manual through the molded process. It is because the compaction is done through a
digital process at constant speed. Cement type C1 has a lower compressive stress of the
cement type C2. It is because the content of cement.
133
Figure. 6.15.Mortar of typical compressive stress-strain curves under
forming using mold (M) and extrusion (E) type C1 and C2
The mean stress–strain curves for each cement mortar and fiber composite
are compared and shown in Fig. 6.16. It can see clearly that the stress–strain
curves of the fiber composite provide better performance than cement mortar.
Figure. 6.16.Mortar and composite of typical compressive stress-strain curves

under forming using mold (M) and extrusion (E)
The evolution of stress and strain in tensile strength and compressive

strength are shown in the figure 6.17. Extrusion process affects the mechanical
performance of materials compared to the mold that results obtained an increase
of almost two times is 183% for the compressive strength while the tensile
strength obtained increase in two and a half time is 257%.
134
Figure. 6.17. Compressive and tensile of stress-strain curves of mortar under
forming using mold (M) and extrusion (E)
Figure 6.15 to 6.17 gives an indication that the processes of forming by

extrusion provide performance results of compressive strength, and tensile
strength is better than the manual process with mold.
6.5. Failure modes.
Failure modes in extruded of cement mortar and coir fiber reinforced

cementitious composites (CFRCC) are reviewed during the compression test and
splitting tensile test. Observations made with photograph and micrograph
6.5.1. Failure modes in compression
The failure modes of typical compression failure modes of cement mortar type
C1 without fiber: (a) extruded plain mortar; (b) after static loading shown in
Figure 6.18. Moreover, the typical compression failure modes of extruded cement
mortar type C2 non-fiber shown figure 6.19. Failure modes are lighter than
cement mortar type C1.The mortar without fibers resulting test sample was
destroyed at the top.
135
Figure 6.18.Typical compression failure modes of cement mortar type C1
without fiber: (a) extruded plain mortar; (b) after static loading.
Figure 6.19.Typical compression failure modes of extruded cement mortar

type C2 non-fiber: (a) plain mortar; (b) after static loading.
The failure compression of static loading, composite 4% fiber type C1 and

C2 as shown in Figure 6.20 are present the failure mode with cracked lengthwise
direction unidirectional pressure and can be seen for cracks on the bottom and top
surface. The detailed information on the failure modes of the coir fiber reinforced
cementitious composites based on fiber content was shown in Figure 6.21. of
failure compression of static loading: (a) composites 4% fiber, (b) composites 3%
fiber, (c) composite 2% fiber. The crack marked has a tendency to propagate
parallel to the loading direction in the mortar matrix. Fiber content increases the
tendency of cracks that occur less and less. Then, it shows the strength of the fiber
bond with mortar matrix.
136
Figure 6.20.Photograph of failure compression of static loading,
composite 4% fiber: (a) type C1 and (b) type C2
Figure 6.21.Photograph of failure compression of static loading: (a)

composites4% fiber, (b) composites 3% fiber, (c) composite 2% fiber.
Figure 6.22 shows the bond between the fiber and matrix mortar. There are fibers
that are pulled out from the mortar, fiber breaking due to the pressure, and fiber is
still immersed in the mortar. It shows the direction of fibers in the mortar is
random. To more clearly for coir fiber reinforced cementitious composites are
137
shown in Figure 6.23 composite failure after compression of static loading, for
broken fiber transverse and longitudinal directions.
Figure 6.22. Micrograph coir fiber reinforced cementitious composites, after

failure compression of static loading.
(a) (b)
Figure 6.23. Micrograph composite after failure compression of static loading,
for broken fiber.
6.5.2. Failure modes in tension
The failure modes of typical tension failure modes under static loading: (a)
cement mortar type C1 non-fiber; (b) cement mortar type C2 non-fiber is shown
in Figure 6.24. The failure mode of cement mortar type C2 is more brittle than the
type C1. It is influenced by the amount of cement and clay.
Typical tension failure modes under static loading of coir fiber reinforced
cementitious mortar composites are shown in Figure 6.25. The existence of fiber
affects the cracks that occur in the mortar. Bonding fibers to make the cement
mortar tensile strength increases.
138
Figure 6.24.Typical tension failure modes under static loading: (a)
cementitious non-fiber type C1; (b) cementitious non-fiber type C2.
Figure 6.25.Typical tension failure modes under static loading of coir fiber
cementitious composite.
The detailed information on the failure modes of the coir fiber reinforced
cementitious composites based on fiber content was shown in Figure 6.26. of
failure modes of split tensile strength: (a)composite with 2% fiber, (b) composite
3% fiber, (c) composite 4% fiber. The crack marked has a tendency to propagate
parallel to the loading direction in the mortar matrix.
Failure mode at 2% fiber content is shown in the picture 6.26a. The

cracked direction parallels to the direction of loading. Cracks that occur less than
the cracking that occurs in 4% fiber content in the figure 6.26b. That due to
resistance tensile strength at 4% fiber content is higher than the tensile strength of
2% fiber content.
139
Figure 6.26.Failure modes of split tensile strength: (a)composite with 2%
fiber, (b) composite 3% fiber, (c) composite 4% fiber.
Results cracked due to the tensile strength of coir fiber orientation to the
longitudinal direction of extrusion coir fiber reinforced cementitious composites
as shown in Figure 6.27. Fiber orientation looked random and disconnected and
pulled out of the mortar as shown in Figure 6.28. Coir fiber reinforced
cementitious composites, after the failure of static tension loading.
Figure. 6.27. Coir fiber orientation longitudinal direction of extrusion of coir

fiber cement clay mortar composites.
Figure 6.28. Micrograph of CFRCC composite, after the tensile failure of

static loading.
140
More detailed results for bonding fibers in mortar matrix as in Figure 6.29
coir fiber after the failure of static tensile loading, for broken fiber. In the picture
6.29a, had the mark of the fiber is lost, and fiber drawn out mortar. In the figure,
6.29b seemed disconnected fibers condition and seemed to mortar attached and
united with the cross section of the fiber.
(a) (b)
Figure 6.29. Micrograph coir fiber after the tensile failure of static loading,
for broken fiber.
6.6. Mechanical models
6.6.1. Compressive strength behavior
The maximum stress value of stress–strain curves is taken as compressive

strength. Figure 6.30 shows the influence of fiber content on stress. The highest
stress value of stress–strain curves is taken as compressive strength. The straight
line is the stress of cement mortar without fiber. Compressive stress increased
with fiber content.
The empirical model is developed to predict compressive stress based on a

linear trend line obtained with increasing fiber content defined as shown in
equation 6.1.
141
……….…………… (6.1)
Where: is the Compressive stress (MPa); is the fiber content (%); is the
shape parameter (MPa), is reference stress parameter (MPa). The parameters
values of the compressive stress versus fiber content for the tested materials is
shown in Table 6.1. The compressive of CFRCC compared to cement mortar, it
shown an addition of fiber can increase the compressive stress up to 41%.
Table.6.1. Fitting parameters values of the compressive stress versus fiber

content for the tested materials
Parameter Parameter
Fiber length Correlation
(mm) coefficient
(MPa) (MPa)
5 0.9901 1.179 14.222
10 0.9783 1.624 13.639
15 0.9903 1.942 13.602
The relationship between fiber length and alpha parameter is shown defined
Equation 6.2:
……….…………… (6.2)
Furthermore, the models are developed to predict compressive stress based on

fiber content and fiber length defined is shown in equation 6.3:
……….…………… (6.3)
where: is the Compressive stress (MPa); is the fiber length; is the fiber
content (%); is the reference stress parameter (MPa).
142
Figure. 6.30. Effect of fiber content on compressive stress
Figure 6.31 shows the influence of fiber length on a average maximum of

stress. The fiber length of 15mm with a fiber content of 4% gives the highest
value compared to cement mortar without fibers. Compressive stress increases
with increasing fiber length. It is the same as for 4 cm coir fiber length the results
presented by Baruah and Talukdar, (2007). However, the results obtained Ali et
al. (2012) is the compressive strength decreases with increasing fiber for fiber
length 2.5 cm; 5 cm; 7.5 cm. That caused by the creation of air voids because of
long fibers with relatively high fiber content.
Figure. 6.31. Effect of fiber length on compressive stress
143
6.6.2. Tensile strength behavior
The effect of fiber content and fiber length on tensile stress is shown in
Figure 6.32 and Figure 6.33. The tensile stress increases with higher fiber content
and fiber length. The empirical model is developed to predict tensile stress is
based on a linear trend line obtained with increasing fiber content as shown in
equation 6.4.
……….…………… (6.4)
Where: is the tensile stress (MPa); is the fiber content (%); is the shape
parameter (MPa), is reference stress parameter (MPa). The parameters
values of the tensile stress versus fiber content for the tested materials as shown in
Table 6.2. The tensile stress of CFRCC compared to cement mortar, an addition of
fibers can increase the tensile stress up to 39%.
Table.6.2. Fitting parameters values of the tensile stress versus fiber content
for the tested materials
Parameter Parameter
(mm) coefficient
(MPa) (MPa)
5 0.9654 0.216 2.032
10 0.9994 0.248 2.046
15 0.9973 0.305 2.011
The relationship between fiber length and alpha parameter is shown defined
Equation 6.4:
……….…………… (6.5)
Furthermore, the models are developed to predict tensile stress based on fiber
content and fiber length defined is shown in equation 6.5:
……….…………… (6.6)
Where: is the tensile stress (MPa); is the fiber length; is the fiber content
(%); is the reference stress parameter (MPa).
144
Figure. 6.32.Effect of fiber content on tensile stress
Figure 6.33 shows the influence of fiber length on a maximum of stress. The fiber
length of 15mm with a fiber content of 4% gives the highest value compared to
cement mortar without fibers. Tensile stress increases with increasing fiber length.
It is the same as the results presented by Baruah and Talukdar, (2007). However,
the fiber length of more than 2.5 cm the results obtained Ali et al. (2012) getting
splitting tensile strength decreases with higher fiber content.
Figure. 6.33. Effect of fiber length on tensile stress
145
6.6.3. Compressive modulus behavior
Figure 6.34 shows the influence of fiber content on the static modulus of
elasticity due to the compressive strength. The compressive modulus of CFM
composite increased with increasing fiber content. However, the compressive
modulus of CFM composites having 10 mm fibers length increasing fiber contents
showed it first decreased and then increased to 4%, These values were higher than
that of cement mortar. Compared to cement mortar value an addition of fibers
caused about 15% increase for 5mm fibers length of the elastic modulus of CFM
composite. The empirical model is developed to predict compressive modulus
defined as:
……….…………… (6.7)
Where: Ec is the compressive modulus (GPa); is the fiber content parameter of the
values of 0, 1, 2, 3, 4 (%) , ,
are fitting parameters (GPa) corresponding to
fiber length. The fitting parameters values of the compressive modulus versus
fiber content for the tested materials as shown in Table 6.3. The results
polynomial Equation (6.7) is the same as the results obtained by Ali et al. (2012).
Table.6.3. Fitting parameters values of the compressive modulus versus fiber

Parameter Parameter Parameter
(mm) coefficient
(GPa) (GPa) (GPa)
5 0.9996 0.053 0.242 1.828
10 0.9990 0.488 -2.266 3.888
15 0.9918 0.123 -0.323 2.332
146
Figure. 6.34.Effect of fiber content on compressive modulus.
Figure 6.35 shows the influence of fiber length on the static modulus of
elasticity due to the compressive strength. The elastic modulus of CFRCC having
5mm increased with increasing fibre content. However, the compressive modulus
of CFRCC having 10 mm fibres length with decreasing fibre contents showed it
first decreased and then increased to 4%, and these values were higher than that of
cement mortar. Compared to cement mortar value, an addition of fibers caused
about 72% increase for 5mm fibers length of the elastic modulus of CFRCC. The
solid straight line is elastic of cement mortar.
Figure. 6.35. Effect of fiber length on compressive modulus.
Figure 6.36, Figure 6.37 and Figure 6.38 shows the influence of fiber
content on the static modulus of elasticity and the compressive stress for 5mm,
10mm and 15 mm fiber length.
147
Figure. 6.36. Effect of fiber content on compressive stress and compressive
modulus for fiber length 5mm.

148
Figure 6.39 shows the relationship between the compressive stress and
compressive modulus on the fiber content and fiber length. The elastic modulus of
CFRCC increased with increasing fibre content and increased compressive stress.
That is attributed to the improvement of the fiber ability to delay the micro-crack
formation and to arrest crack propagation [Sahmaran et al., 2007]. According to
the research results obtained Ali et al. (2012) modulus of elasticity declined to
fiber length is greater than 5cm and with added fiber.

modulus
149
6.6.4. Tensile modulus behavior
Figure 6.40 shows the influence of fiber content on the static modulus of
elasticity due to the tensile strength. The tensile modulus of CFRCC decreased
with increasing fiber content. However, a tensile modulus of CFRCC having 10
mm fibers length with increasing fiber contents showed it lowest tensile modulus
than that cement mortar. Compared to cement mortar value an addition of fibers
caused about 45% decrease for 10mm fibers length of the tensile modulus of
CFRCC for 4% fiber content.
The empirical model is developed to predict tensile modulus of elasticity

as shown in equation 6.8 and the fitting parameters values of the tensile modulus
versus fiber content for the tested materials as shown in Table 6.4
……….…………… (6.8)
where: Et is the tensile modulus (GPa); is the fiber content (%); , are
fitting parameters (GPa) corresponding to the fiber length.
Table.6.4. Fitting parameters values of the tensile modulus versus Fiber

(mm) coefficient
(GPa) (GPa) (GPa)
5 0.9977 0.014 -0.141 0.956
10 0.9977 0.042 -0.328 1.107
15 0.9912 0.0004 -0.064 0.897
150
Figure. 6.40.Effect of fiber content on tensile modulus.
Figure 6.41 shows the influence of fiber length on tensile modulus of

elasticity due to the tensile strength. The elastic modulus of fiber composite
having 5mm to 15mm decreased with increasing fibre content.
Figure. 6.41.Effect of fiber length on tensile modulus.
However, the compressive modulus of CFRCC having 10 mm fibres

length with increasing fibre contents showed it values were lowest than that of
cement mortar. Compared to cement mortar value, an addition of fibers caused
about 45% decrease for 10mm fibers length of the tensile modulus of CFRCC.
The solid straight line is the elastic modulus of cement mortar. Figure 6.42, Figure
6.43 and Figure 6.44 shows the influence of fiber content on tensile modulus and
the tensile strength for 5mm, 10mm and 15 mm fiber length. Results showed that
the increase in fiber content will increase the tensile stress, but lowers the value of
the tensile modulus.
151
Figure. 6.42.Effect of fiber content on tensile stress and tensile modulus for
fiber length 5mm.
fiber length 10mm.
fiber length 15mm.
Figure 6.45 shows the relationship between the tensile stress and tensile
modulus on the fiber content and fiber length. The tensile modulus of CFRCC
decreased with increasing fibre content and increased tensile stress. It is attributed
to the improvement of the fiber ability to delay the micro-crack formation and to
arrest crack propagation [Sahmaran et al., 2007].
152
6.6.5. Density behavior
Figure 6.34 and Figure 6.35 shows the effect of fiber content and length on
the density of CFRCC. The solid straight line indicates the density of cement
mortar. The presence of fibers content increase and the density only slightly
changes. Also due to the amount of fiber, it can be justified by the effects
experienced by the material in the pressure gradient during its formation. This
pressure gradient matrix porosity overcomes problems caused by the fibers.
However, a decrease in density could be due simply to the low mass volumes of
coir fiber. The density of CFRCC decreased with higher fiber content and
increased with shorter fiber length but still below the cement mortar.
The empirical model is developed to predict density as shown in equation

6.9 and the fitting parameters values of the density versus fiber content for the
tested materials as shown in Table 6.5
……….…………… (6.9)
3
where: is the density (kg/m ); is the fiber content (%); , are fitting
3
parameters (kg/m ) corresponding to the fiber length.
153
Table.6.5. Fitting parameters values of the density versus fiber content for the
tested materials
(mm) coefficient
(kg/m3) (kg/m3) (kg/m3)
5 0.9992 -2.907 0.545 2122.9
10 0.9866 0.409 -21.306 2142.4
15 0.9791 3.773 -47.452 2166.1
In general, the density of fiber composite in 4% fiber content decreased up

to 3.9% for 15mm; 2.6% for 10mm; 2 % for 5mm as compared to that of cement
mortar as shown in Figure 6.46. As well as shown in Figure 6.47, the density of
fiber composite in 15mm fiber length decreased up to 3.8 % for 4% fiber content;
3.3% for 3% fiber content; 1.3% for 2% fiber content as compared to that of
cement mortar.
Figure. 6.46.Effect fiber content on density
154
Figure. 6.47.Effect fiber length on density
Figure 6.48, Figure 6.49 and Figure 6.50 shows the influence of fiber
content on density and the tensile strength for 5mm, 10mm and 15 mm fiber
length. Results showed that the increase in fiber content will increase the tensile
strength, but lowers the value of the density. Same as obtained by Ali et al. (2012)
to get the density of composite decreased with higher fiber content and increased
with shorter fiber length.
length 5mm.
155
length 10mm.
length 15mm.
Effect of fiber content on density and tensile stress for fiber length are
shown in Figure 6.51. Tensile stress increases with increasing fiber content while
density decreases. Also, due to the amount of fiber, it can be justified by the
effects experienced by the material in the pressure gradient during its formation.
This pressure gradient matrix overcome porosity problems caused by the fibers.
Furthermore, the density of the CFRCC decrease by an increase of fiber added,
leading to an improvement in strength/weight ratio.
156
length.
6.6.6. Strain Behavior
Figure 6.52 and Figure 6.53 shows he experimental test results the effect
of fiber content and length on the strain of CFRCC, under forming using
extrusion. The solid straight line indicates a strain of the cement mortar. Strain
value increases with increasing the fiber content. The value of strain with 10mm
fiber length gives a higher value than the fibers length of 15mm, and it is above
the value of the strain of cement mortar.
The empirical model is developed to predict strain as shown in equation

6.10 and the fitting parameters values of the strain versus fiber content for the
tested materials as shown in Table 6.6
……….…………… (6.10)
where: is the tensile strain (%); is the fiber content (%); , are fitting
parameters (%) corresponding to the fiber length.
157
Table.6.6. Fitting parameters values of the tensile strain versus fiber content
for the tested materials
(mm) coefficient
(%) (%) (%)
5 0.9965 -0.001 0.047 0.3145
10 0.9983 -0.052 0.427 -0.0123
15 0.9705 -0.033 0.242 0.1569
Figure. 6.52. Effect fiber content on strain
Figure 6.53 shows the influence fiber length on strain due to the tensile
stress. The strain of CFRCC for 10 mm fiber length has a higher value than the
strain at 5 mm and 15 mm fiber length. Strain value increased with increasing
fibre content.
158
Figure. 6.53.Effect fiber length on strain
Effect of fiber content on strain and the tensile stress for 5mm, 10mm and
15 mm fiber length was shown in Figure 6.54, Figure 6.55 and Figure 6.56.
Results showed that the increase in fiber content will increase strain and the
tensile stress.
Figure. 6.54.Effect of fiber content on tensile stress and strain for fiber length
5mm.
159
10mm.
15mm.
Effect of fiber content on tensile stress and strain for fiber length are
shown in Figure 6.57. The tensile stress and strain increase with increasing fiber
content. The strain for 10mm fiber length higher strain value of the fiber length of
5mm and 15mm. The fiber length of 10mm gives a higher strain value of the fiber
length of 5mm and 15mm. The increase in strain reached 142% of the strains
cement mortar. While the tensile stress increased by 40% from the strain of
cement mortar
160
6.7. The conclusion of the chapter.
The performance mechanical of coir fiber reinforced cement mortar

composites compared with cement mortar. Moreover, information obtained
where structural composite materials are an excellent opportunity to produce
components that achieve weight savings and improved properties. Fiber
reinforced cementitious material can enhance by processing, such as extrusion
that will improve the interfacial bond through the application of pressure.
Mechanical performance tensile and compressive strength can be

improved through the process of surface treatment of fibers and after going
through the extrusion process for compacting with a smooth surface result that the
materials are extrudability.
Aspects surface obtained as a result of the mold in comparison with the

outcome of the screw extrusion process. Mold process is uneven, not smooth
surface defects as well as the extrusion process. In observation of the composite
material obtained fiber direction lengthwise direction is random. The processes of
161
forming by extrusion provide performance results of compressive strength, and
tensile strength is better than the manual process with mold.
Tensile strength and compressive strength of mortars have shown a

gradual increase in increasing fiber content and fiber length. These values are
higher for fiber composites when compared to cement mortar ones. The empirical
model is developed to predict compressive strength and tensile strength based on a
linear trend line obtained with increasing fiber content defined as:
The models are developed to predict compressive stress based on fiber

content, and fiber length defined as:
The models are developed to predict tensile stress based on fiber content
and fiber length defined as:
Compressive modulus of CFRCC increased with the increasing fiber

content and increased compressive strength while the tensile modulus of coir fiber
cement mortar composites decreased with increasing fiber content and increased
tensile strength. The empirical model is developed to predict compressive
modulus and tensile modulus defined as:
Density decreases with the increasing fiber content, increased the

compressive strength and tensile strength. The empirical model is developed to
predict density with increasing fiber content defined as:
The tensile strain and tensile strength increases with the increasing fiber
content. The strain for 10mm fiber length has higher strain value of the fiber
length of 5mm and 15mm. The empirical model is developed to predict strain with
increasing fiber content defined as:
162
The failure mode for mortar with cracked lengthwise direction
unidirectional pressure and can be seen for cracks on the bottom and top surface.
The mortar without fibers resulting test sample destroyed at the top. The failure
mode for composites that the crack marked has a tendency to propagate parallel to
the loading direction in the mortar matrix. Fiber content increases the tendency of
cracks that occur less. It shows the strength of the fiber bond with mortar matrix.
163
CHAPTER.7.
MICROMECHANICS, MICROSTRUCTURE,
DAMAGE AND MODELS OF SCREW EXTRUDED
FIBER COMPOSITES USING NONDESTRUCTIVE
TESTING METHOD
7.1. Introduction
In this section, the following deals with characteristic, damage,

micromechanics and modeling of the cement mortar and coir fiber reinforced
cementitious composite mortar (CFRCC) using digital image correlation (DIC),
nondestructive method. Results of the microstructural examination, using an
optical microscope and scanning electron microscope (SEM). It is shown that the
shape of the pore, the distribution and orientation of coir fiber determines the
compressive and tensile behavior of the composite. In the present investigation,
the maximum compressive and tensile strengths are observed for composite
containing coir fiber and hence the discussion based on this composition. The
compressive parameter strength and tensile strength are very often used to
quantify the quality of cementitious materials.
7.2. Mechanical characteristics of fiber composite behavior
The mechanical properties of extruded cement mortar and extruded

CFRCC obtained from the DIC technique are presented in this section.
Compressive strength and tensile strength are processed with Aramis -3D
software. The specimen used cylindrical for compressive and splitting tensile test.
7.2.1. Compressive strength behavior
The axial deformation of cement mortar and fiber composite was recorded
using DIC method. The strain of the front surface of the fiber composite measured
with the DIC system by stacking images obtained at different stages of loading.
The stress–strain curves measured by MTS and DIC method showed good
agreement as displayed and compared in Figure 7.1 for cement mortar and Figure
7.2 for fiber composite.
164
The axial strain at the beginning introduced due to the vertical
deformation. The cement mortar that did not contain coarse aggregates exhibited
the almost uniform deformation before the peak load.
Figure. 7.1. Typical compressive stress – strain curves of cement mortar

using MTS and DIC
The peak load from the compressive strength showed a lower value in the
cement mortar compared to the fiber composite. It indicates that the stiffness of
cement mortar appears relatively lower than those of fiber composite. However,
the cement mortar having the strain higher than the CRFCC, because the cement
mortar have a long time for failure and due to effect clay in a mortar.
Figure. 7.2. Typical compressive stress – strain curves of fiber composite

using MTS and DIC
When compared to the fiber composite then cement mortar as shown in
Figure 7.3. Stress value of the fiber composite higher than the cement mortar.
165
That is because of the contribution of fiber strength. However, the strain of the
cement mortar is greater than the fiber composite for compressive strength
testing.
Figure. 7.3. Typical compressive stress – strain curves of fiber composite

using MTS and DIC
7.2.2. Tensile strength behavior
Observation of the tensile strength through the splitting tensile strength

measurement using the MTS contact method and by DIC no contact method as
shown in Figure 7.4 and Figure. 7.5. show approximately equal results.
Figure. 7.4. Typical split tensile stress – strain curves of cement mortar
using MTS and DIC
166
The load value can retain by the CFRCC is twice that of the load obtained
by cement mortar. That is because in the case of cement mortar cracks in the
matrix. However, cracks occur in the CFRCC material after the defense of the
fiber. Also, when viewed from a failure of the CFRCC materials have nearly
twice the time of the failure of the cement mortar. Thus, the addition fibers made
of ductile properties for CFRCC materials.
Figure. 7.5. Typical split tensile stress – strain curves of fiber composite
using MTS and DIC
Figure 7.6 shows the stress value of the fiber composite is higher than the
cement mortar. As well as strain value of composite after the peak load has higher
strain than the strain of the cement mortar. The CFRCC strain reached 5% while
on cement mortar reaches 3%. That is due to the effect of the strength of the fiber
that is ductile.
Figure. 7.6. Typical split tensile stress – strain curves of fiber composite
using MTS and DIC
167
7.3. Damage Evolution.
Digital Image Correlation (DIC) are used to investigate the damage

processes of cement mortar and CFRCC under compressive strength and tensile
strength. Strain and displacement were computed to analyze the initial cracks and
propagation during loading.
The compressive and tensile characteristics of extruded CFRCC were

determined by testing a minimum of three-cylinder specimens for each batch
using the Mechanical Testing System (MTS) and the Digital Image Correlation
(DIC). The accuracy of displacement and strain measurements obtained. DIC
technique depends on the quality of speckle pattern, surrounding vibrations,
lighting, out-of-plane displacements and specimen height used for strain
computations. [Shah et Chandra Kishen, 2011]. The displacement contour maps
obtained from the DIC system can show detailed crack patterns. On the other
hand, the small strain concentrations distribution can provide information about
the micro cracks initiation and development [Van Mier, 2008]
On the contrary, the deformations in the fiber composite and cement

mortar which stemmed from the growth of microcracks and failure of interfacial
bonds show continuous increase through the whole pre-peak range. Hence, the
failure processes in these specimens started from a very early loading stage and
developed gradually with the increase of loading. During the pre-peak loading
phase, the lateral deformation of fiber composite was more evident than that of
cement mortar. It indicates that there are more micro cracks in the fiber composite
than cement mortar within the pre-peak loading range.
We will now describe the strain and displacement distribution of CFRCC

composite obtained from DIC method at different stages of loading and the strain
contour maps obtained from DIC measurement system at four phases are elastic,
inelastic, plastic and failure.
7.3.1. the compressive strength of extruded composites
The evolution of the compressive behavior of extruded CFRCC can divide

into four phase (elastic, inelastic, softening and failure).
168
7.3.1.1 Elastic stage
Figure.7.7. Shows the evolution of apparent normal strain in the elastic

region during the compression for fiber composite. It shows typical displacement
and strain distribution contour. During this stage, reaching 30% of the maximum
loading no cracks has occurred.
Figure. 7.7. Evolution of apparent normal strain during the compression at

the elastic region for fiber composite.
7.3.1.2 Inelastic
Figure . 7.8. Presents the strain distribution contour of CFRCC at the

inelastic region, 30%-100% of peak loading. At this stage, initial microcracks
occurred in 50% of the maximum load. Cracks spread following the spread of
cracks to the highest load of 100%; Fiber began to pull out from the matrix and
then disconnected. With the increase of loading, the cracks did not uniformly
develop on the specimen surface, which locally concentrated and grew vertically.
Figure. 7.8. Evolution of apparent normal strain during the compression

during inelasticity phase for fiber composite.
169
7.3.1.3 Softening stage
In the softening region, fibers worked up at 20% after the peak load. In
this conditions, basic cement mortar failure occurs, fibers are pulled out, broken,
and the matrix collapsed, as shown in Figure 7.9. It is observed that a crack
initiated at the peak load and propagated in the loading direction at the post-peak
range. The main crack propagated almost over the whole height of the sample test.
Figure. 7.9. Evolution of apparent normal strain at selected points during the
compression at inelastic after peak load for fiber composite.
7.3.1.4 Failure
After softening phase, the global failure occurs to crack propagates along
the direction of loading and then load drop and sample failure. Although, the
sample is still standing thanks to the remaining bridges of fibers into the matrix.
Figure. 7.10. Evolution of apparent normal strain at selected points during

the compression at failure for fiber composite
170
7.3.2. Composites extruded on tensile strength
The evolution of the damage by the splitting test in quasi -static loading
can be divided into three phases: elastic, failure and post failure. The initial crack
occurs after the peak load
7.3.2.1 Elastic
Figure.7.11. It shows the evolution of apparent normal strain in the elastic

region. It shows typical displacement and strain distribution contour. In this
region, no cracks occur.
Figure. 7.11. Evolution of apparent average strain during the splitting tension
static loading at elastic for fiber composite.
7.3.2.2 Peak load
Figure 7.12. Shows the strain distribution at the peak load. Initial crack is
instantaneous along the diameter and corresponds to the load drop. In this
condition, a tensile strength between the fiber composite and cement mortar
matrix occurs until leading to the fiber pull-out and breakage. The failure
171
processes of fiber composite under tensile strength showed a linearly elastic
behavior until peak. The fiber composite showed better post-peak behavior than
cement mortar.
Figure. 7.12. Evolution of apparent average strain during the splitting tension
at peak load for fiber composite.
7.3.2.3 Post-failure stage
Figure 7.13. Presents damage evolution after peak load and load drop until
55% of peak load. In this region, cracks propagated and then fiber pulled out from
the matrix and broke up. It first occurred in the middle of the outer side of the top
and bottom. Failure occurs when the center of the crack has reached the top of the
sample loading location.
The tensile of the CFRCC has a value of the displacement of the one and
half time of the compressive. Also, the residual strength 50% of the maximum
load after load peaks. This condition of the CFRCC is suitable for application to
the pavement and drainage pipelines.
172
Figure. 7.13. Evolution of apparent normal strain during the splitting
tension at plastic for fiber composite
173
7.4. Microstructure
The microstructure was observed using the scanning electron micrographs

(SEM). It showed void formation on the mortar surface at the fracture surface;
fiber fracture were also seen in the crack growth direction and interfacial
transition zone.
7.4.1. Fractography
Fractography of extruded CFRCC after failure under static loading

produced by SEM given in Figure. 7.14. It is showing the existence of apparent
voids due to the fiber pull-out detected despite the existence of certain partial
bonding between large microfibers and mortar matrices. In general, the fault
occurs inside, after the resistance of the fiber. Some of the fibers appear to break
up, there is a strong attachment to the fiber and mortar. Noticeably, the crack
growth came from the direction of loading and then surrounds the fiber.
Figure.7.14. Fracture surface under static loading on splitting tensile of

extruded CFRCC of SEM micrograph (50x magnification).
Furthermore, after a 200x magnification, as shown in Figure 7.15. SEM

showed after the break up of coconut fiber resistance between fiber and matrix.
Thus breaking occurs in the mortar after the withdrawal of the fiber. The growth
of small cracks is also observed in the mortar surface zone. The CFRCC strength
is partially bearded by the bond between the fiber and the mortar.
174
under static loading of extruded CFRCC
There is also a broken fiber surface evenly with the mortar, as illustrated in
figure 7.16. After a 500x magnification that looks broken fiber regularly, without
any part of the fiber cells out of the fiber.

Also, the conditions are shown in Figure 7.17 disconnected fiber, which
previously occurred due to the withdrawal of ductile fibers. At the end of the
fiber, show the fiber cells fused due to strain.
175
Figure.7.17. SEM micrograph (500x magnification) of the fiber fracture
7.4.2. Interfacial transition zone.
Figure 7.18 shows the relationship between fibers and mortar after the
failure of the CFRCC. The interfacial transition zone (ITZ) of CFRCC under
static loading by SEM 500x magnifications is shown in figure 7.18. It shows the
micro cracks in the mortar and gap which exist at the fiber-mortar interfacial zone.
As the test results in the failure processes of the CFRCC shown, bond
cracks first appeared around the weak interfacial transition zone and then
propagated into the mortar regions. Moreover, the micro cracks locations, sizes,
and shapes in the interfacial transition zone were influenced by the relative
strength of the mortar matrix. As a result, the observable cracks appeared at both
the old interfacial transition zone and new interfacial transition zone. Also, the
cracks development of fiber composite depends on the relative strength of fiber
and mortar. When the force of the fiber is weaker than that of mortar, the cracks
probably go through the fiber in CFRCC. It implies that the relative strength
significantly influences the failure mode of CFRCC.
176
Figure.7.18. SEM micrograph (500x magnifications) of the fracture surface of
CFRCC after static loading.
Meanwhile, fiber embedded in the mortar after failure in the interfacial

transition zone of CFRCC under static loading by SEM 500x magnifications is
shown in figure 7.19. It shows that the matrix and the fibers are strongly bonded.
In general, the microstructure studies suggest that a strong bond exists between
the fiber and the matrix /mortar.
Figure.7.19. SEM micrograph (500x magnifications) of the fracture surface of

CFRCC after static loading.
177
7.5. Micromechanical models.
An analytical approach based on micromechanical models is proposed.

The analytical approach using the rule of the mixture (ROM) is a micro-
mechanical based approach used for approximate estimation of CFRCC
properties. It base on an assumption that a fiber composite property is the volume
weighted average of its constituent properties, fiber, and mortar. Micromechanical
models permit to study the tensile strength and compressive strength of the
composite material. The analytical model approach confronted with the
experimental results.
7.5.1. Micromechanical models for tensile strength.
For fiber composite materials in which the reinforcement fiber is subject to

much higher stresses (σf >> σm,) than the matrix and there is a redistribution of
the load. Theoretical calculations of the tensile strength in the longitudinal
direction were conducted using the rule of mixtures (the two contributions
assuming m + f = 1, i.e. no voids or other inclusions):
σtc = σtm ( 1- f ) + σf f …………………… (7.1)
where, σtc is tensile strength of composites (MPa), σtm is tensile strength of

mortar (MPa), σf is tensile strength of fiber (MPa), and f is fiber volume
fraction (described in equation (7.2) and (7.3)).
……………………….. (7.2)
……………….. (7.3)
Modified rule of the mixture is often used to predict the strength of short
fiber composites [Shao and Bernd, 1996]. This method considered two other
factors that will affect the properties of composite materials which is fiber
orientation and fiber length. Hence, it is also applied to estimate the performance
of the specimens too. The equation (7.1) for tensile strength applied to fiber
composites The formulas are given equation (7.4.).
σtc = σtm f) + ηL ηO σf f ……………………..… (7.4)
178
Where, ηL is the fiber length distribution factor (ηL =1 for fibers longer than
about 10mm), and ηo is the fiber orientation distribution factor (ηO =0.2 for fibers
random 3D).
The experimental tensile strength results were obtained by carried out
splitting tensile strength test by DIC and MTS. the comparison made between The
ROM value using equations (7.4) and experimental value to evaluate the validity
of the theoretical outcome. The tensile strength of CFRCC using equation (7.4)
need calibration coefficient for fiber content (Cf) to signification with
experimental. The results obtained for f = 0.04 is Cf =0.45; for f = 0.06 is Cf
=0.55; for f = 0.08 is Cf =0.85. For CFRCC using equation (7.4), proposed
tensile strength fiber composite models with calibration coefficient for fiber
content (Cf) is modified rule of mixture (MROM) as shown in Equation (7.5):
σtc = Cf ηL ηO σf f + σtm f) ……………………..… (7.5)
Figure 7.20 showed the predicted and experimental tensile strength of

different fiber volume fraction. The tensile strength value of CFRCC by MROM
is less approaching the experiments value. R-square value = 0.8626 can be
expressed following equation (7.6):
σtc = 18.129 f + 1.7664……..…….….….…….. (7.6)
Figure. 7.20. The tensile strength versus fiber volume fraction.
Summerscales et al.,(2011),(2013) proposed for the elasticity modulus that

a fiber diameter distribution factor should be included in ROM. Virk et al., (2012)
also proposed the fiber area correction factor for elasticity modulus. The law
179
states that the composite tensile strength (σtc) should account for both the tensile
strength of the cement mortar/plain matrix (σm) and the tensile strength of fiber (σf
), wich is a contribution from the fibers (length Lf , diameter df and fiber volume
fraction f ). Taking into account the ratio of fiber (Lf / df), the proposed models
development Equation (7.5) as follows Equation (7.7):
σtc = Cf ηl ηo ( Lf / df ) f σf + σtm ( 1- f ) ………………..… (7.7)
The results have been obtained relationship of tensile strength (σtm) to

compressive strength (σcm) of cement mortar in this study proposed as shown in
Equation (7.9):
σtm = ……………………..… (7.8)
By entering equation (7.8), the proposed models of equation (7.7) can be

expressed:
σtc = Cf ηl ηo ( Lf / df ) f σf + ( 1- f ) ………………..…
(7.9)
The tensile strength results obtained with the proposed models equation
(7.9) for signification with experimental results. The results of the CFRCC
obtained for f = 0.04 is Cf =0.11; for f = 0.06 is Cf =0.075; for f = 0.08 is Cf
=0.07.
The results comparison tensile strength of fiber composite between the
experimental results (MTS method and DIC method) with the proposed modified
the rule of mixture (MROM) (Equation (7.5)) and proposed model (Equation
(7.9)) as shown in Figure 7.21.
180
Figure. 7.21. Relative tensile strength as a function of the fiber factor for
modification the model predictions.
For fiber factor versus relative tensile strength of CFRCC is shown in

Figure 7.21 the following equations are proposed equation (7.10):
(R-square value = 0.9645) …………………..…

(7.10)
To change σtm it can show as follows equation (7.11):
.….….… (7.11)
Equation (7.10) is in good agreement with the relative tensile strength test data
shown in Figure. 7.21. For different values.
The tensile strength of CFRCC is observed from experimental and model

is shown in Figure 7.20-21, increased with volume fraction irrespective of
the mix type, a similar observation were done on Portland cement based fiber
composites (Tasse ST and Lubell AS, 2014).
181
7.5.2. Micromechanical models for compressive strength
Observation and analysis of the model of the compressive strength of the

CFRCC based micromechanical model is a rule of the mixer. It is as has been
done to produce a compressive strength composite model. The compressive
strength of a composite (σcc) material can normally be predicted using the
standard rule-of-mixtures in the longitudinal direction were conducted using the
rule of mixtures models is shown in equation (7.12):
σcc = σcm m + σf f ……………………..… (7.12)
Theoretical calculations of the compressive strength in the longitudinal

direction were conducted using the rule of mixtures (the two contributions
assuming m + f = 1, i.e. no voids or other inclusions):
σcc = σcm f) + σf f …………………… (7.13)
where, σcc is the compressive strength of composites (MPa), σcm is the

compressive strength of mortar (MPa), σf is compressive strength of fiber (MPa),
and f is fiber volume fraction.
Modified rule of the mixture is often used to predict the strength of short
fiber composites [Shao and Bernd, 1996]. This method considered two other
factors that will affect the properties of composite materials which is fiber
orientation and fiber length. Hence, it is also applied to estimate the performance
of the specimens too. The equation (7.13) for compressive strength applied to
fiber reinforced composites The formulas are given equation (7.4.).
σcc = σcm f) + ηL ηO σf f ……………………..… (7.14)
Where, ηL is the fiber length distribution factor (ηL =1 for fibers longer than
about 10mm), and ηo is the fiber orientation distribution factor (ηO =0.2 for fibers
random 3D).
The experimental compressive strength results were obtained by carried

out compressive strength test by DIC and MTS. The comparison is made between
The ROM value using equations (7.14) and experimental value to evaluate the
validity of the theoretical result. The compressive strength of fiber composite
using equation (7.14) need calibration coefficient for fiber content (Cf) to
signification with experimental. The results obtained for f = 0.04 is Cf =0.45; for
f = 0.06 is Cf =2.5; for f = 0.08 is Cf =4.5. For CFRCC using equation (7.14),
182
proposed compressive strength fiber composite models with calibration
coefficient for fiber content (Cf) is modified rule of mixture (MROM) as shown in
Equation (7.15):
σcc = Cf ηL ηO σf f + σcm f) ……………………..… (7.15)
Figure 7.22 showed the predicted and experimental tensile strength of

different fiber volume fraction. The compressive strength value of CFRCC by
MROM is less approaching the experiments value. R-square value = 0.8006 can
be expressed following equation (7.16):
σcc = 84.4 f + 15.034……..…….….….…….. (7.16)
Figure. 7.22. The compressive strength versus fiber volume fraction.
Summerscales et al.,(2011),(2013) proposed for the elasticity modulus that

a fiber diameter distribution factor should be included in ROM. Virk et al., (2012)
also proposed the fiber area correction factor for elasticity modulus. The law
states that the composite compressive strength (σcc) should account for both the
tensile strength of the cement mortar / plain matrix (σcm) and the fiber, wich is a
contribution from the fibers (length Lf , diameter df and fiber volume fraction f ).
Taking into account the ratio of fiber (Lf / df), the proposed compressive strength
fiber composite models development Equation (7.15) as follows Equation (7.17):
σcc = Cf ηl ηo ( Lf / df ) f σf + σcm ( 1- f ) ………………..… (7.17)
183
The compressive strength results obtained with the proposed models
equation (7.17) for signification with experimental results. The results of the
CFRCC obtained for f = 0.04 is Cf =0.45; for f = 0.06 is Cf =0.40; for f =
0.08 is Cf =0.35.
The results comparison compressive strength of fiber composite between

the experimental results (MTS method and DIC method) with the proposed
models is modified the rule of mixture (MROM) is Equation (7.15) and developed
MROM is proposed model be Equation (7.17) as shown in Figure 7.23.
Figure. 7.23. Relative compressive strength versus the fiber factor for
modification the model predictions.
For fiber factor versus relative compressive strength of CFRCC is shown

in Figure 7.23 the following equations are proposed equation (7.30):
(R-square value = 0.9437) …………. (7.18)
Equation (7.18) is in good agreement with the relative tensile strength test data
shown in Figure. 7.23. For different values.
184
It is observed from Figure 7.22-23 that compressive strength increased
with increases in volume fraction irrespective of the mix type. A similar
observation as Portland cement based fiber composites ( Tasse ST and Lubell AS,
2014).
7.5.3. Comparison between models and experimental results
Two analytical approaches namely the standard rule of the mixture and
developed model of the CFRCC properties were proposed. Analytical approaches
were compared with experiment data from the MTS and the DIC results. They are
presented in Table 7.1 for tensile strength and Table 7.2 for compressive strength.
It shows the theoretical tensile strength values calculated from the modified rule
of mixtures model and developed the model, along with the experimental values
using MTS and DIC. Experimental strength values of composites with fiber
contents of 2%, 3%, and 4% were approximately 95% of the analytical model.
It can be observed from the table that the model results are closer to the
experimental for the case of tensile strength and compressive strength. For tensile
strength, the experimental and analytical results for MTS and MROM do not
compare very well. However, proposed model, MROM, and the experimental
result of DIC compare very well. Unlike the case with the compressive strength,
the experimental and analytical results are much closed.
Table.7.1. Comparison tensile strength of fiber composite properties obtained

from experiment and analytical model.
Values tensile strength (MPa)
Parameters Experiment Analytical model
Tensile strength for MTS DIC Modified Proposed
composite Rule of model
σtc mixture
(MROM)
Cement Mortar 2.2966 1.9116 1.9116 1.9116
Fiber composite 2%
2.6483 2.3886 2.2808 2.4323
fiber content
Fiber composite 3%
2.9293 2.9037 2.6066 2.6966
fiber content
CFM Composite 4%
3.2198 3.5019 3.4098 3.2235
fiber content
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Table.7.2. Comparison compressive strength of fiber composite properties
obtained from experiment and analytical model.
Values compressive strength (MPa)
Parameters
the compressive Experiment Analytical model
strength of the MTS DIC Modified Proposed
composite Rule of model
σcc mixture
(MROM)
Cement Mortar 15.5451 15.7201 15.7990 15.7990
Fiber Composite 2%
17.0220 16.8334 17.6483 17.6182
fiber content
Fiber Composite 3%
19.7809 17.0555 18.5463 19.6612
fiber content
CFM Composite 4%
21.1966 25.3200 23.2966 21.8812
fiber content
Validation is done with the relationship between the experimental and

analytic models. Figure 7.24 showing y = 0.9611x + 0.0216, R² =
0.992 and Figure 7.25 showing y = 0.9803x + 0.0117, R² = 0.9987
respectively for tensile strength and compressive strength are shows the same
correlation approach.
Figure. 7.24. Model versus experimental tensile strength for the CFRCC
186
Figure. 7.25. Model versus experimental compressive strength for the CFRCC
The study results indicate that the discrepancy between the tensile strength
of coir fiber and mortar matrix significantly influences the mechanical properties
and crack patterns of the composites materials. The findings in this investigation
are useful to improve the mechanical properties of CFRCC by optimizing the mix
proportion with extrusion.
It found that the damage process is related to the relative strength of fiber
and mortar matrix. The observation implies that the propagations of microcracks
are different between composites and plain mortar. The compressive strength and
tensile strength results all indicated that the fiber failure mode was predominantly
by fracture fiber rather than pull out, even for the shortest fibers in use in this
study.
The global cracks developed along the loading direction for all the
cement-based materials. For cement mortar, the first crack appeared surface
mortar and then propagated into the mortar region to the load direction. In fiber
composite, the initial cracks occurred around interfacial transition zone and
propagated across the mortar region connecting with each other. Understanding
of the differences in the failure processes between cement mortar and fiber
composite can provide insights into the failure mechanism of concrete. It can use
187
to improve the mechanical properties of concrete through optimization of the
mixture proportions.
A micromechanical analytical model of the fiber composite is developed

based on the micromechanics. Based on the analysis, the following conclusions
can be obtained. Developed new rules of the mixture have proposed which
introduce additional length and diameter fiber parameters. The models proposed
for fiber composite is the tensile strength and compressive strength of the
mechanical properties. The model proposed in this paper accepts micromechanical
parameters of fiber and mortar; it can be used to predict the tensile strength and
compressive strength of fiber composite.
The general model prediction defined as:
σcc = Cf ηl ηo ( Lf / df ) f σf + σcm ( 1- f ) (for compressive strength)
σtc = Cf ηl ηo (Lf / df) f σf (1- f ) (for tensile strength)
The analytical model is developed to predict tensile strength of the CFRCC

defined as:
The analytical model is developed to predict compressive strength of the

CFRCC defined as:
The develop rule of the mixture models was successfully used to relate the
tensile strength and compressive strength with fiber volume and length The
experimental result demonstrates the validity of the proposed model is agreement
close. The DIC results and MTS result compared with the models destructive
testing results; they compared very well.
188
CHAPTER.8.
GENERAL CONCLUSIONS AND FURTHER RESEARCH
8.1. Conclusions.
This study developed new fiber composite materials for a structural element of
the screw extruded with the local materials that are cement, clay, sand and coir fiber,
which can use for building construction. It was designed to investigate the properties of
coir fiber, cement mortar, and composites on fresh state and hardened state using MTS
and DIC testing method. Also, it observed the microstructure by SEM and developed
analytical models for the yield stress of rheology, mechanical and micromechanical.
The related conclusions are summarized as follows:
A. Physical, mechanical performances, and microstructure of coir fibers
1. The treatment of coir fibers increases the tensile strength and delivers higher
value to the elongation of a break than the ones of untreated fibers. Average
tensile strength of treated fiber is as twice greater than the one of untreated.
Based on these results, coir fiber after treatment presents an improved ductile.
Indonesian coir fiber has ductile properties suitable for use as reinforcement in
concrete composites with high ductility.
2. The treatment significantly removes impurities on the fiber surface, resulting in
surface modification and improved thermal stability. TGA measurements
revealed that the treatment of fibers has a positive impact on the thermal stability
of the sample.
3. SEM observation shows that water treatment has a significant impact of on the
surface of the fibers (removing impurities, decreasing the siliceous compounds
content) and decreases the average diameter of the fibers. These changes in fiber
structure induce an improvement of the macroscopic behavior of the fibers.
B. Design, rheology properties, microstructure and rheology model of product

extruded composites.
1. This present work shows that yield stress model used for common mortar can be
generalized to fiber reinforced concretes. Indeed, it is the evolution of the yield
stress of fiber-reinforced cementitious composite.
2. Rheological behaviors of mortar and composites reinforced with fibers are
presented. The formation of cement clay material through extrusion produces a
compact material with the material surface without defects.
189
3. The rheological approach is an effective design guide of fresh cement mortar to
achieve hardening properties of the composite. The rheology is important for the
characteristic of fresh cement mortar performing in practical applications. It is
used for achieving the desirable properties of the hardened materials
4. The formulation of a material with low cement and from local materials that can
extrude with smooth and compact is studied. Clay absorbs more water than
cement. Therefore, the amount of clay and water/cement ratio is added to the
mortar will influence the extrusion results.
5. Mix design mortar obtained from cement, clay and sand in the ratio of the
weight of 1:3:6 respectively require 18 % water/cement. As for the proportion of
2:2:6 it need a 16 % water/cement to produce the extruded material.
6. The addition of fibers into extruded formulations, the calculation, required the
addition of water/cement ratio, to obtain an extruded mortar well and to counter
the loss of workability due to the addition of the selected fiber into mortar
mixture basic (plain mortar) without adding extra water.
7. The addition of fibers up to 5 % by weight of cement, to remain in the extruded
condition, for 10 % of cement formulations need water/cement ratio of 21 %. As
for the 20 % cement formulations needed water/cement ratio of 19 %.
8. Rheology properties show that the value of the torque increases with decreasing
amount of water and the yield stress increases with fiber content and fiber
length.
9. Rheology models for CFRCC composites have been obtained. The model
rheology of prediction yield stress is as follows:
The model predictions the yield stress show good agreement with the yield stress
values experiment.
10. The SEM observations of the CFRCC before extrusion was the small holes and
not spread between the mortar and fibers, due need extrusion in order to fiber
spread more evenly and compact between fiber and mortar.
C. Mechanical performance, microstructure, and models of screw extruded

composites using destructive testing method
1. The performance mechanical of the CFRCC compared with cement mortar is

presented. Fiber reinforced cementitious composite can enhance by processing,
such as extrusion, which improve the interfacial bond through the application of
pressure.
190
2. Aspects surface is obtained as a consequence of the mold in comparison with the
outcome of the screw extrusion process. Mold process is uneven, not smooth
surface defects compare than the extrusion process.
3. The SEM observation of the composite material obtained fiber direction
lengthwise direction is random.
4. The processes of forming by extrusion provide performance results of
compressive strength, and tensile strength that is better than the manual process
with mold.
5. Tensile strength and compressive strength of mortars have shown a gradual
increase in increasing fiber content and fiber length. These values are higher for
CFRCC composites when compared to cement mortar ones.
6. The empirical model is developed to predict compressive strength and tensile
strength based on a linear trend line obtained with increasing fiber content
defined as:
7. The models are developed to predict compressive stress based on fiber content,
and fiber length defined as:
8. The models are developed to predict tensile stress based on fiber content and
fiber length defined as:
9. Compressive modulus of CFRCC increased with the increasing fiber content and
increased compressive strength while the tensile modulus of coir fiber cement
mortar composites decreased with increasing fiber content and increased tensile
strength.
10.The empirical model is developed to predict compressive modulus and tensile
modulus defined as:
11. Density decreases with the increasing fiber content, increased the compressive
strength and tensile strength. The empirical model is developed to predict
density with increasing fiber content defined as:
12.The tensile strain and tensile strength increases with the increasing fiber content.
The strain for 10mm fiber length has higher strain value of the fiber length of
5mm and 15mm. The empirical model is developed to predict strain with
increasing fiber content defined as:
13. The failure mode for the mortar with cracked lengthwise direction unidirectional
pressure can be seen for cracks on the bottom and top surface. The mortar
without fibers results in test sample destroyed at the top. The failure mode for
composites that the crack marked has a tendency to propagate parallel to the
191
loading direction in the mortar matrix. Fiber content increases the tendency of
cracks that occur less. It shows the strength of the fiber bond with mortar matrix.
14. The proposed analytical model for CFRCC composite was found to fit closely
the experimental data points of the stress-strain curve and hence, can use in the
prediction of stress-strain characteristics for concrete structures.
D. Micromechanical, damage evolution, microstructure, and models of screw

extruded composites using nondestructive testing method
1. The study results indicate that the discrepancy between the tensile strength of
coir fiber and mortar matrix significantly influences the mechanical properties
and crack patterns of the composites materials. The findings in this investigation
are useful to improve the mechanical properties of CFRCC by optimizing the
mix proportion with extrusion.
2. It found that the damage process is related to the relative strength of fiber and
mortar matrix. The observation implies that the propagations of microcracks are
different between composites and plain mortar. The compressive strength and
tensile strength results all indicated that the fiber failure mode was
predominantly by fracture fiber rather than pull out, even for the shortest fibers
in use in this study.
3. The global cracks developed along the loading direction for all the cement-based
materials. For cement mortar, the first crack appeared surface mortar and then
propagated into the mortar region to the load direction. In fiber composite, the
initial cracks occurred around interfacial transition zone and propagated across
the mortar region connecting with each other. Understanding of the differences
in the failure processes between cement mortar and fiber composite can provide
insights into the failure mechanism of concrete. It can be used to improve the
mechanical properties of concrete through optimization of the mixture
proportions.
4. A micromechanical analytical model of the fiber composite is developed based
on the micromechanics. Based on the analysis, the following conclusions can
be obtained. Developed new rules of the mixture have proposed which introduce
additional length and diameter fiber parameters. The models proposed for fiber
composite is the tensile strength and compressive strength of the mechanical
properties. The model proposed in this paper accepts micromechanical
parameters of fiber and mortar; it can be used to predict the tensile strength and
compressive strength of fiber composite.
5. The general model for prediction compressive defined as:
σcc = Cf ηl ηo (Lf / df ) f σf + σcm ( 1- f )
192
6. The general model for prediction tensile defined as:
σtc = Cf ηl ηo (Lf / df) f σf (1- f )
7. The analytical model is developed to predict tensile strength of the CFRCC

defined as:
8. The analytical model is developed to predict compressive strength of the

CFRCC defined as:
9. The develop rule of the mixture models was successfully used to relate the
tensile strength and compressive strength with fiber volume and length The
experimental result demonstrates the validity of the proposed model is
agreement close. The DIC results and MTS results compared with the models,
they compared very well.
8.2. Further Research.
Although, the findings important and the model that has been obtained from the
development of new materials in this research, further research is still needed to be done
for more specific characteristics based on this research. The following are the
recommendations for future work:
1. Develop a program of research with the same experimental test that can be
performed and developed using different natural fibers (such as bamboo fiber,
rice fiber, fiber banana leaves) and mortar of different materials.
2. Develop research use fiber treatment with chemicals and refinement of methods
of treatment.
3. Develop an investigation on the effect of fiber on the thermal response, cyclic
load to composite materials.
4. Further investigation of the post-failure analysis using DIC to understand the
damage mechanisms of CFRCC composite material.
5. Study the simulation models to predict the mechanical properties and cracks
with finite element method.
193
6. Apply the results of the research conducted on the construction material
products, such as an ingredient in the manufacture of panel buildings, pavement,
drainage pipes, mortar for concrete, and brick.
194
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APPENDICES
International Journal And Proceeding Published
1. Riana H.Lumingkewas, Heru Purnomo, Gilles Ausias, Dedi Priadi, Thibaut

Lecompte, Arnaud Perrot, Tensile Characteristics of Coconut Fibers Reinforced
Mortar Composites, Advanced Materials Research Vol. 651 (2013) pp 269-273 ©
(2013) Trans Tech Publications, Switzerland,
doi:10.4028/www.scientific.net/AMR.651.269
2. Riana H Lumingkewas, Gilles Ausias, Thibaut Lecompte, Arnaud Perrot, Irwan

Katili, Heru Purnomo, Sigit P Hadiwardoy. Effect of Fibers Content on the Tensile
Properties of Coconut Fibers Reinforced Cement Mortar Composites, Advanced
Materials Research Vol. 742 (2013) pp 92-97 © (2013) Trans Tech Publications,
Switzerland, doi:10.4028/www.scientific.net/AMR.742.92
3. Riana Lumingkewas, Gilles Ausias, Thibaut Lecompte, Arnaud Perrot,

IrwanKatili, HeruPurnomo, Microstructural Properties Of Natural Coconut Fibers-
Based Green Mortar Composites, Proceeding, Journée des doctorants de l‘école
doctorale Santé Information Communication Matière et Mathématiques (SICMA).
Université Européenne de Bretagne. Lorient, France, September, 13th, 2012.
4. Riana H. Lumingkewas, Heru Purnomo, Gilles Ausias, Thibaut Lecompte, Arnaud

Perrot, Dedi Priadi, IrwanKatili. Properties Of Indonesian Coconut Fibers For
Cement-Based Materials Reinforcement, Proceeding, Third international
conference on natural polymers, biopolymers,biomaterials, their composites, blends,
IPNs, Polyelectrolytes and Gels : macro to nano scales (ICNP-2012). Kottayam,
Kerala, India. October 26, 27 &28, 2012.
5. Riana H.Lumingkewas, Heru Purnomo, Gilles Ausias, Dedi Priadi, Thibaut

Lecompte, Arnaud Perrot, Tensile Characteristics of Coconut Fibers Reinforced
Mortar Composites, Proceeding, International Conference Engineering Material
(ICEM 2012) Singapore, Singapore, December 30-31, 2012.
6. Riana H Lumingkewas, Gilles Ausias, Thibaut Lecompte, Arnaud Perrot, Irwan

Katili, Heru Purnomo, Sigit P Hadiwardoyo, Effect of Fibers Content on the Tensile
Properties of Coconut Fibers Reinforced Cement Mortar Composites, Proceeding,
International Conference on Civil, Materials and Environmental Sciences,
Vancouver, Canada, April 17-18, 2013.
7. Heru Purnomo, Dedi Priadi, Riana H Lumingkewas, Strength Improvement of

Early Age Unfired Soil-Lime Bricks, International journal, Advanced Materials
Research Vol. 689 (2013) pp 299-303.
8. Heru Purnomo, Dedi Priadi, Gilles Ausias, Thibaut Lecompte, H. Riana

Lumingkewas, Arnaud Perrot, Effect of Coconut Fibers Addition to early Age
Unfired Soil-Lime Bricks Strength, International Journal, Key Engineering
Materials.Vol.594-595 (2014) pp 471-476
212
ABSTRAK
Name : Riana Herlina LUMINGKEWAS

Study Program: Civil Engineering
Title: Development Of Materials For Construction With Low Environmental
Impact Made With Low Content Of Cement And With Natural
Fibers.
Tujuan dari disertasi ini adalah memberikan kontribusi pada bidang bahan bangunan
untuk industri konstruksi, dengan mengembangkan penelitian tentang bahan bangunan
terbarukan yang ramah lingkungan. Bahan dibuat dengan sedikit semen dan menggunakan
bahan-bahan lokal seperti tanah liat dan limbah serat alam. Pembentukan melalui proses
teknologi ekstrusi. Tujuan jangka panjang untuk menemukan bahan-bahan baru bangunan
ramah lingkungan terbuat dari bahan lokal untuk meningkatkan kualitas kinerja, mempercepat
pembangunan dan mengurangi biaya konstruksi.
Studi pertama dilakukan pemeriksaan sifat fisik, mekanik, termal dan mikro-struktur
serat alam dari sabut kelapa yang banyak tersedia di Indonesia. Kemudian, ditinjau
perbandingan serat sabut kelapa yang melalui perawatan dan tidak dirawat. Selanjutnya,
mengembangkan model Weibull untuk mendapatkan model kekuatan tarik serat tunggal sabut
kelapa. Studi kedua, merancang formula bahan komposit serat sabut kelapa diperkuat semen dan
lempung untuk dapat dibentuk melalui proses teknologi ekstruksi spiral. Setelah itu, pengujian
rheologi digunakan rheometer untuk memeriksa dampak serat pada perilaku semen yang
distabilkan dengan pasta tanah liat. Lalu, dianalisa untuk diperoleh model prediksi tegangan
luluh bahan komposit. Studi ketiga, memeriksa kinerja produk ekstrusi secara mekanik,
menggunakan metode destruktif dengan sistem pengujian mekanik (MTS) dan menggunakan
metode pengujian non destruktif dengan korelasi citra digital (DIC). Lalu, dikembangkan model
mekanikal dan mikromekanikal serat komposit. Untuk mendapatkan karakterisasi komponen
mikro pengujian dengan Scanning Electron Microscope (SEM). Evolusi kegagalan dan
kerusakan bahan diamati retak mikro.
Hasil yang diperoleh dari studi ini, kinerja serat dapat ditingkatkan melalui perawatan
serta didapatkan model kekuatan tarik serat tunggal. Selanjutnya, didapatkan formula produk
ekstrusi bahan mortar serat komposit yang dapat diekstruksi tanpa cacat pada permukaan.
Diperoleh juga model reologi untuk memprediksi tegangan luluh serat komposit. Penambahan
serat sabut kelapa meningkatkan kekuatan tekan dan tarik dibandingkan tanpa serat. Evolusi
Kegagalan dan kerusakkan bahan serat komposite lebih tangguh dari pada bahan normal.
Didapat pula model mekanikal akibat efek serat dan model mikromekanikal tekan dan tarik dari
serat komposit. Model yang dihasilkan dibandingkan dengan hasil data eksperimen MTS dan
DIC, memberikan hasil adanya kesesuaian. Bahan bangunan yang dihasilkan merupakan bahan
ramah lingkungan, daktail dan sangat cocok untuk bangunan di daerah gempa.
.
Kata kunci: serat alam, rheology, ekstrusi, mekanikal, mikrostruktur, damage, DIC.
213
RESUME

Study Program : Civil Engineering
Title : Développement de matériaux pour la construction à faible impact
environnemental Fait à faible teneur en ciment et de fibres naturelles
Le but de cette thèse est de contribuer au domaine des matériaux de construction pour
l'industrie de la construction, en développant la recherche sur les matériaux de construction
renouvelables qui sont respectueux de l'environnement. Matériaux fabriqués avec un peu de
ciment et en utilisant des matériaux locaux tels que l'argile et des déchets de fibres naturelles.
Formation dans le processus de la technologie d'extrusion. Objectif à long terme de trouver de
nouveaux matériaux de construction respectueux de l'environnement à partir de matériaux
locaux pour améliorer la qualité de la performance, d'accélérer le développement et de réduire
les coûts de construction.
La première étude a examiné la structure de microphysique, mécanique, thermique et de
fibres naturelles de noix de coco qui est largement disponible en Indonésie. Puis, en termes de
rapport en fibres de coco et que grâce à un traitement non traités. En outre, le développement de
modèles de Weibull pour obtenir des modèles d'une seule résistance à la traction de la fibre de
coco. La deuxième étude, la formule conçue de coco matériaux composites de ciment renforcés
de fibres et de l'argile doit être formée par un processus de technologie de l'extrusion en spirale.
Après cela, le test rhéologique rhéomètre utilisé pour examiner l'incidence sur le comportement
de la pâte de ciment de fibres stabilisé avec de l'argile. Ensuite, analysé pour obtenir des
modèles prédictifs de la limite d'élasticité des matériaux composites. La troisième étude,
inspecter les performances du produit d'extrusion mécanique, en utilisant destructrice système
de test mécanique (MTS) et en utilisant des méthodes d'essais non destructifs avec corrélation
d'image numérique (DIC). Ensuite, développé des modèles micromécaniques des fibres
mécaniques et composites. Pour obtenir la caractérisation des tests micro composants par
microscope électronique à balayage (MEB). L'évolution de l'échec et de dommages matériels
observé microfissures.
Les résultats obtenus de cette étude, la performance de la fibre peut être améliorée par
un traitement et ont obtenu un seul des modèles de résistance à la traction de la fibre. En outre,
les produits d'extrusion de la formule mortier obtenu des matériaux composites de fibres
peuvent être extrudés sans défauts sur la surface. Aussi obtenu modèles rhéologiques pour
prédire le rendement des composites de fibre de contrainte. Ajout de la fibre de coco augmente
la résistance à la compression et à la traction que sans fibres. L‘évolution de défaillance et de la
destruction du matériel de fibre composite est plus résistant que le matériau normal. De même
dérivé des effets de modèles et des modèles de micromécanique robinet de fibres et traînée de
composites de fibres mécaniques. Le modèle résultant est comparé avec les résultats des
données expérimentales MTS et DIC, donnant les résultats de leur pertinence. Le matériau de
construction qui en résulte est des matériaux écologiques, ductiles et très approprié pour les
bâtiments dans les zones sismiques
Mots-clés: fibres de coco, extrusion, rhéologie, mécaniques, dommage, micromécanique.
214
ABSTRACT

Study Program: Civil Engineering
Title: Development of Environmentally Friendly Materials for
Construction Made With Low Content of Cement and With Natural
Fibers
The purpose of this study is to contribute to the field of building materials on
concrete technology for the construction industry, by developing research on renewable
building materials that are environmentally friendly. Materials are made with low
cement and using local materials such as clay, sand, and waste natural fiber, formation
through the process of extrusion technology. The long-term goal is finding new green
building materials of natural fiber reinforced cementitious composite to improve the
quality of performance, speed up the building and reduce construction costs.
The first study examined the physical, mechanical, thermal and microstructure
of natural fibers of coir fiber that is widely available in Indonesia. Then, in terms of coir
fiber ratio treated and untreated. The second study, designed the formulation of coir
fiber reinforced cementitious composite materials to formed through a process of the
screw extrusion technology. After that, rheological testing rheometer used to examine
the behavior of fiber cement paste stabilized with clay. Then, it analyzed to derive
predictive models of the yield stress of fiber reinforced cementitious composite
materials. The third study, inspect mechanical extrusion product performance, using
Mechanical Testing System (MTS) and using non-destructive testing methods with
Digital Image Correlation (DIC). Then, develop mechanical models and
micromechanical models. To get the characterization of micro-components are testing
by Scanning Electron Microscope (SEM).
The results obtained from this study, the performance of coir fiber can be
improved through treatment. Furthermore, the formula obtained extrusion products coir
fiber cementitious composite materials can extrude without defects on the surface. Also,
it obtained rheological models to predict the yield stress. The addition of coir fiber
increases the compressive strength and tensile strength than the normal concrete.
Similarly, it obtained mechanical models of the fiber effects and micromechanical
models of compressive strength and tensile strength of the fiber cementitious composite.
The resulting model compared with experimental data results of MTS and DIC, are
giving significant results.
Keywords: coir fibers, extrusion, rheology, mechanical, micromechanical.
215

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Development of Fiber Concrete

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présentée par

THESE / UNIVERISTE DE BRETAGNE SUD

Development of Materials Thèse soutenue le //2015

for Construction with M. Dedi PRIADI

Low Environmental M. Irwan KATILI

Content of Cement and Professeur, Université de Cergy- Pontoise / Examinateur

The research reported in this dissertation was a part of cooperation between

(Riana Herlina Lumingkewas-Hadiwardoyo)

CHAPTER.6. ...................................................................................................................................... 124

CHAPTER.7. ...................................................................................................................................... 164

CHAPTER.8. ...................................................................................................................................... 189

REFERENCES ................................................................................................................................... 195

APPENDICES .................................................................................................................................... 212

ABSTRAK .......................................................................................................................................... 213

Figure.2.1. Stress versus percentage strains of various fibers ............................ 14

Figure.3.1. The flow chart of the research design ................................................. 47

Figure. 4.1. Untreated coir fiber ............................................................................ 72

Figure. 7.1. Typical compressive stress – strain curves of cement mortar

Table.2.1 Chemical composition of some natural ﬁbers ...................................... 10

Table 3.1 Chemical composition of cement.......................................................... 57

Table.5.1. Mixture proportions of cement, clay, and sand.................................... 99

Table.6.1. Fitting parameters values of the compressive stress versus fiber

Table.7.1. Comparison tensile strength of fiber composite properties

1.1. Research background

Recently, researchers are extremely focused toward the global warming.

Use of natural fibers in cementitious composites is an alternative in

The material ingredients of the cementitious composite are similar to that of

The incorporation of such natural fibers as cement and/or earth-based materials

Processing can substantially influence fiber dispersion and orientation, material

1.2. Research Question

Currently, developments of new building material products focused on

1.3. Objective of research

1.4. Limitation of Research.

Based on the above background, there is an urgency to develop new building

1.5. Contribution of Research

1.6. Overview of Dissertation

This dissertation is divided into eight chapters, as follows:

The first chapter contains an introduction describing the background and

In the fourth chapter, an analysis of the performance of natural fibers from

The seventh chapter consists in the development of a micromechanical model

This state of the art on construction materials focused on the properties

The mechanical performances of such composites studied at micro and

2.2. Natural Fiber

Natural fibers represent a renewable resource that is available almost all

Furthermore, due to cancer health risks [Azuma 2009], it is now forbidden

2.2.1. Structure and chemical composition.

The principal components of the fiber cell walls are cellulose,

Lignin is an amorphous and heterogeneous mixture of polymer and

Table 2.1 Chemical composition of some natural ﬁbers

Cellulose Hemicellulose Lignin Waxes

Bagasse 55.2 16.8 25.3 –

Rice husk 35–45 19–25 20 14–17

2.2.2. Physical and mechanical properties

Many factors can influence mechanical properties of natural fibers. First, it

Table 2.2 Physical-mechanical properties of natural fiber

Abaca 400 12 3–10 1.5

Oil palm 248 3.2 25 0.7–1.55

Pineapple 400–627 1.44 14.5 0.8–1.6

Coir 175 4–6 30 1.2

Source: [Faruk 2012]. Has been reprocessed