Heat Treatment of Files
Heat Treatment of Files
Heat Treatment of Files
A b s t r ac t
The use of nickel–titanium (NiTi) alloys created a revolutionary impact in endodontic treatments. Shape memory and superelastic property of an
NiTi alloy make the instrument more flexible, which improves the quality of the treatment by reducing the procedural errors. Even though these
instruments show advanced metallurgical properties, it can lead to fracture due to fatigability. To improve the fracture resistance and enhance
the clinical performance, various thermomechanical heat treatments had been introduced to these NiTi instruments. NiTi alloy undergoes phase
transformation on heat treatment to upgrade the mechanical properties. This review article appraises the improved metallurgical properties
of NiTi alloy by various thermomechanical heat treatment processes in addition with discussion of recently introduced thermomechanically
altered NiTi endodontic instruments.
Keywords: Austenite, Cyclic fatigability, Edge endo files, Martensite, Nickel–titanium alloy, Phase transformation, R-phase.
Conservative Dentistry and Endodontic Journal (2019): 10.5005/jp-journals-10048-0047
I n t r o d u c t i o n 1
Department of Conservative Dentistry and Endodontics, Sree
Nickel–titanium alloys (NiTi) have been popularly used in Mookambika Institute of Dental Sciences, Coimbatore, Tamil Nadu,
endodontic practice because of its more desirable and enhanced India
2–4
metallurgical properties over stainless steel instruments. Shape Department of Conservative Dentistry and Endodontics, Sree
memory and superelastic property of NiTi alloy allow the material Mookambika Institute of Dental Sciences, Kanyakumari, Tamil Nadu,
more flexible, which makes a significant improvement in working India
of rotary endodontic instruments. Usage of NiTi alloys in engine- Corresponding Author: Loganathan Ashok, Department of Conserv-
driven endodontic instruments will reduce the procedural errors ative Dentistry and Endodontics, Sree Mookambika Institute of Dental
when compared to stainless steel instruments. In spite of advanced Sciences, Coimbatore, Tamil Nadu, India, Phone: +91 9003308879,
metallurgical properties, NiTi instruments still prone for fracture e-mail: [email protected]
during root canal instrumentation. Two types of fracture can occur How to cite this article: Ashok L, Krishnan V, Nair RS, et al. An Overview
in NiTi instruments, flexural fracture and torsional fracture.1 During of Thermomechanically Heat-treated Nickel–Titanium Alloy Used in
Endodontics. Cons Dent Endod J 2019;4(2):34–38.
instrumentation in curved canals, NiTi instruments undergoes
flexural fracture due to increased cyclic fatigability. Torsional Source of support: Nil
fracture occurs when repeated loading and unloading of instrument Conflict of interest: None
leads to repetitive phase transformation within the material.
Application of stress over the instrument will lead to microstructural
changes that in turn cause phase transformation, which can be material to revert to its original shape on heating due to phase
controlled by several thermomechanical treatments of the alloy. The transformation of stable-deformed martensite to stable austenite
recently introduced thermomechanically treated NiTi instruments phase. Superelastic effect is completely recoverable elastic state
show improved fracture resistance and it has created a revolutionary between stable austenite to stress-induced martensite phase
impact on the mechanical properties, which improves the clinical due to phase transformation. 2 This molecular transition allows
performance in rotary endodontics. the material to become flexible without undergoing permanent
deformation.
N i c k e l –T i ta n i u m A l loys Conventional NiTi wires transform from parent austenitic phase
NiTi alloy composed of nickel (56%) and titanium (44%). NiTi alloy to distorted rhombohedral crystal structure on heating under
was named NITINOL after it was developed by the Naval Ordinance certain conditions. This phase is called intermediate R-phase.
Laboratory. Alloy exists in two different phases depending on Austenitic alloy is hard when compared to martensitic alloy and
crystal structure. shows superior superelastic property. Martensitic alloy is soft and
ductile and shows shape memory effect, because of this property,
• Austenitic phase which is a parent phase with cubic B2 crystal
it exhibits increased cyclic fatigue resistance than austenitic alloy
structure.
(Fig. 1).
• Martensitic phase with monoclinic B19 crystal structure.
If the transformation temperature is above austenitic finish
When stress is applied, it undergoes phase transformation temperature (Af ), then the alloy is in austenitic state. On cooling,
from austenitic phase to martensitic phase, which exhibits shape if the temperature goes below the martensitic finish temperature
memory and superelastic property that ascertain the uniqueness (Mf ), then the alloy is in martensitic phase or daughter phase.2 This
of the alloy. Shape memory effect is the ability of the deformed transformation is also called as military transformation.
© The Author(s). 2019 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (https://creativecommons.
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Nickel–Titanium Alloy Used in Endodontics: A Review
Fig. 1: Hysteresis of austenitic (parent) phase to martensitic (daughter) Fig. 2: NiTi phase transformation (Courtesy: Thompson SA. Int Endod J
phase transformation (Courtesy: Zupanc J. Int Endod J 2018;51: 2000;33:297–310)
1088–1103)
by factors including chemical composition, heat treatment, and
Shear type process induced in the martensitic phase of an alloy, method of manufacturing. Flexibility of the instrument can be
which gives rise to twinned martensite that forms the structure of a increased by phase transformation on heat treatment that can
closely arranged hexagonal lattice.3 The original martensite shape improve the metallurgical properties of NiTi files by increasing the
can be deformed easily to a single orientation structure detwinned cyclic fatigue resistance.6
martensite by a process called detwinning. Martensitic phase possesses Electropolishing is an electrochemical process of removing
more ductile behavior than the austenite phase. The deformation can the surface irregularities and microcracks formed during grinding
be reversed by heating the alloy above the temperature transformation process. This will increase the fracture resistance and resistance to
range called reverse temperature transformation range (RTTR). corrosion of the instrument.7
The thermoelastic behavior of a martensitic alloy can thrive
either by a temperature variation called thermally induced A u s t e n i t i c A l loy
martensite (TIM) or by the application of stresses which in turn
High flexibility of the instruments is one of the major advantages of
result into strains is called strain-induced martensite (SIM) (Fig. 2).
NiTi alloys. When stress is applied to the instruments, it possesses
Modulus of elasticity describes the stiffness of the material.
superelastic property that can undergo reversible deformation of
The modulus of elasticity of martensitic alloy is 30–40 GPa which is
the instrument. To utilize superelastic property in NiTi endodontic
lower than that of austenite, which shows the modulus of elasticity
instruments, the alloy should be in parent austenitic phase.8
in the range of 80–90 GPa.2 R-phase shows modulus of elasticity
lower than that of martensite.
C o n v e n t i o n a l N i T i W i r e s
F r ac t u r e o f N i T i A l loys Conventional NiTi alloys are in the austenite phase at room
To minimize the iatrogenic procedural errors during root canal temperatures. Activation of austenitic NiTi produces an elastic
instrumentation, the use of stainless steel instruments had deformation that follows a linear stress/strain function. If stress-
overcome by NiTi alloy instruments. Despite its flexibility, fracture of induced deformation increases, the superelastic deformation
these instruments is one of the major problems in clinical practice. appears, whereas strain remains constant. This superelastic behavior
Reason for fracture is mainly due to incorrect or over usage of is a direct consequence of the martensitic transformation, which
instruments.4 Two types of fracture can occur in NiTi instruments: (1) occurs at the crystallographic level. Conventional NiTi instruments
torsional fracture and (2) flexural fracture. Torsional fracture usually include Mtwo, OneShape, ProFile, and ProTaper Universal.
is the result of an intense tensional force that has been applied to
the instrument. This means the continuous loading and unloading M- wi r e
of instruments produces a high stress tension that may be superior A proprietary thermomechanical processing can be done to
to the 8% allowed by the alloy that causes unrecoverable plastic improve the cyclic fatigue resistance of the rotary NiTi instruments
deformation and leads to fracture.1,5 and to develop M-wire technology. Because of its unique
Flexural fracture occurs due to cyclic fatigue of the instrument. nanocrystalline martensitic microstructure, M-wire have higher
When the instrument is subjected to repeated cycles of compression strength and wear resistance than similar instruments made of
and tension, cyclic fatigue failure occurs. According to Martin and conventional superelastic NiTi wires (Ye and Gao).9 According
DiBernardo, after loading is applied to the instrument and analyzed to Alapati et al., the austenite finish temperature of M-wire was
using scanning electron microscope (SEM), the files begin to show found to be around 43–50°C and this clearly shows it was well
irreversible microcrack formation on the alloy crystallographic above austenitic finish temperature of conventional NiTi and body
structure. These microcracks lead to crack propagation process temperature, indicating that under clinical conditions, M-wire is
and contribute to failure.5 not completely composed of austenite.10 M-wire contains phases
Phase transformation behavior plays an important role in that are in both the deformed and microtwinned martensitic,
mechanical properties of Ni–Ti instruments and is easily influenced R-phase, and are austenite whilst maintaining a pseudoelastic state.
The examples of M-wire instruments include Dentsply’s ProFile GT transformation. The amount of this transformation is a function of
Series X, ProFile Vortex, ProTaper Next files, Path Files, WaveOne, the start (Ms) and the finish (Mf ) temperatures. This is the reason
and Reciproc (VDW, Munich, Germany). The R-phase and martensitic for the alloy possesses shape memory effect. Shear type of process
phase elastic modulus is lower than that of austenitic phase, and induces the transformation that occurs in the alloy, which leads to
because of the presence of these phases in M-wire, it tends to be change in its metallurgical properties, which forms a new phase
more flexible, thus shows improved cyclic fatigue resistance. The called the martensitic or daughter phase which in turn gives
M-wire had physical and mechanical properties that can make the rise to twinned martensite that forms the structure of a closely
instruments more flexible and fatigue resistant than those made packed hexagonal lattice. This martensite shape can be deformed
with conventionally processed NiTi wires.11 easily to a single orientation by a process known as detwinning
to detwinned martensite when there is a “flipping over” type of
R- p h a s e shear. 3 The additional property of the instrument in deformed
The R-phase is an intermediate phase, a rhombohedral distortion martensitic phase is if the alloy is heated beyond the austenite finish
of the cubic austenitic phase (Fig. 3), with one of the four directions temperature (e.g., autoclaving), it will return back to its original
of the cubic austenite stretched.12 shape by returning to the primary austenitic state. Martensitic phase
The austenite to R-phase transformation is martensitic and is of NiTi alloy is more soft and ductile than the austenite phase.2
easily reversed by heating. Further, it introduces very small volume
changes and can be self-accommodated by combining twin-related CM W i r e
variants. This transformation is thermoelastic and has all the typical
CM wire was introduced by DS Dental in 2010. To increase the
characteristics of a shape memory alloy, including shape memory
flexibility, reduce the shape memory, raise the transformation
and superelasticity (Fig. 3).
temperatures (Af to about 50°C), and to obtain stable martensite
Leandro and his colleagues evaluated the mechanical property
at the body temperature of the NiTi alloy, a thermomechanical
of R-phase using finite element analysis (FEA). They concluded
heat treatment is processed over the alloy. According to Testarelli
that the R-phase instrument showed the highest flexibility when
et al., the nickel composition of CM wires has lower percentage in
compared with other instruments. The R-phase demands a lower
weight when compared to conventional NiTi alloy. CM wires exhibit
moment to be applied on an instrument during bending until 45°.
martensitic phase with varying amounts of austenite and R-phase.
The R-phase instrument shows the highest angular deflection in
The controlled memory effect helps the endodontic instrument
response to a torque of 3 N/mm when torsional force is applied.
to retain the shape of the canal even when it is taken out from the
This shows that the presence of R-phase in the alloy increases the
canal. This property helps avoid procedural errors such as ledge
flexibility but decreases the torsional stiffness of the endodontic
formation, transportation, and perforations. The extreme flexibility
instrument. The results from FEA study shows that the R-phase
and less taper of these files show increased fatigue resistance in
instrument presents the lowest stress values under bending,
curved canal cases.15 Hyflex CM, Hyflex EDM, and Thypoon Infinite
which is expected when a lower moment is required to bend an
Flex NiTi files are the examples of CM wire.
instrument. Thus, the same material presented stresses only on
the surface during the torsional simulation. In spite of the larger
deformation imposed on this instrument during torsion, its core is H yf l e x CM
preserved from the damaging effects of this loading condition.13 The Af temperature of CM wire (Hyflex CM and Typhoon CM) is
R-phase instruments show similar cyclic fatigue resistance in around 47–55°C, which is above the intracanal temperature.16 Hyflex
comparison with those made of M-wire.14 CM wires show increased flexibility, high fatigue resistance, and
Twisted file, twisted file adaptive, and K3XF (not twisted) are improved cutting efficiency when compared to electropolished
the examples of R-phase wires. and conventional NiTi instruments.2,17 In the study of Shen et al.,
the higher Af temperature of CM instruments was consistent with
M a r t e n s i t i c A l loy a mixture of austenite, R phase, and martensite structure. Hyflex
The unique characteristic of NiTi alloy that when it is cooled through
a critical transformation temperature range (TTR), changes in
modulus of elasticity, yield strength, and electric resistivity occur
as a result of changes in electron bonding (Fig. 4).
By decreasing the temperature through this range, which leads
to a change in the crystal structure is known as the martensitic
CM files have unique characteristic of rewinding of the file after instruments contain both martensitic (20°C) and austenitic (35°C)
autoclaving, and if the file does not rewind, it indicates that it needs phases. Currently, two max wire (martensite-austenite-electropolish
to be discarded.16,17 file X) instruments are available commercially XP-endo shaper and
XP-endo finisher. These files are introduced by FKG Dentaire in 2016.
H yf l e x EDM Max wire instruments possess martensitic stable phase at room
Hyflex electrical discharge machining (EDM) is manufactured using temperature. When it is placed inside the canal due to intracanal
the technique of EDM. Electrical discharge machining is also known temperature changes, it transforms the phase into austenitic state.
as spark machining or spark eroding. It is a noncontact thermal Thus, it exhibits both shape memory and superelastic property and
erosion process used to machine electrically conductive materials changes its shape according to change in intracanal temperature.
using controlled electrical discharges to attain a desired shape. The These instruments show improved torsional resistance during
electrical sparks used as a cutting tool cause a local melting and erode preparation in curved canal. On comparison with TRUShape
small portions of workpiece to produce crater-like surface finish. Both instruments, XP-endo shaper instruments showed a higher cyclic
cutting tool and workpiece embedded in a dielectric liquid and voltage fatigue resistance and angle of rotation to fracture but lower torque
are applied. The metal removal is accomplished by pulsed electrical to failure.21 The Af temperature of XP-endo shaper files is around
discharge. The ionized dielectric liquid removes the metal and 35°C. XP endo finisher is a new type anatomical finishing file and
produces nondirectional surface finish. This avoids the early instrument consists of a nontapered rotary file of size 25. XP endo finisher R is
failure that results from conventional grinding techniques. After a variation of XP endo finisher file designed for retreatment cases.22
cutting and cleaning, the instrument placed in a ultrasonics acid bath
and it is heat treated at temperature ranging between 300°C and 600°C
K3 XF
for 10 minutes to 5 hours. The Af temperatures of EDM files is around To increase the cyclic fatigue resistance, R-phase technology had
52°C.1,2,15 According to Shen et al., the fatigue resistance of EDM files is been introduced in manufacturing of NiTi endodontic instruments.
higher than that of CM files.18 The metallographic analysis of new and K3XF was developed by SybronEndo in 2011 which takes advantage
used files shows a homogenous structure and it is mostly composed of R-phase technology. It is fabricated similar to K3 files, but
of lenticular martensite grains and some residual austenite (Pirani), instead of twisting process, these files undergo grinding to attain a
and it shows 700% higher fatigue resistance than CM instruments.19 desired shape. K3XF files are subjected to a special heat treatment
after the grinding process, which enhances the flexibility and
G o l d - t r e at e d and B lu e - t r e at e d strength and also modifies the crystalline structure of the alloy to
accommodate some of the internal stress. K3XF instruments have
I n s t r u m e n ts an Af temperature below the body temperature (37°C). Therefore,
To overcome the defects occurring during machining process and to it has an austenite structure at body temperature and would
modify the crystalline phase structure, new heat treatment method exhibit a superelastic property during clinical application. The
had been recently introduced called postmachining heat treatment. postmachining heat treatment processing used for K3XF modifies
These instruments undergo proprietary thermomechanical heat the transformation temperature by releasing crystal lattice defects
treatment after grinding process.11 The first endodontic instrument and diminishing internal strain energy.1,23
possessing a distinctive blue color was ProFile Vortex Blue. Titanium
oxide layer on the surface after machining process is responsible Edge Endo Files
for distinctive blue color. Commercially, there are two gold-treated EdgeFile (EdgeEndo, Albuquerque, NM, USA) is made of an annealed
instruments, and two blue-treated instruments are available. In that, heat-treated NiTi alloy brand named fire-wire. According to
profile vortex blue and protaper gold are used in rotary. Reciproc manufacturer, edge endo files show extreme durability, incredible
blue and WaveOne gold are used in reciprocating motion. The Af of flexibility, and strong enough to resist forces acting on torsion. Edge
blue treated instruments is around 38.5°C and Ms is around 31°C.16 endo produces three different file systems X3, X5, and X7.24 X3 files
The Af of gold-treated instrument is around 50°C, which indicates are compatible with the settings of ProTaper and ProTaper Next
that these instruments mainly contain martensite or R-phase (Dentsply Tulsa Specialties, Tulsa, OK, USA) rotary file systems. X5
under clinical conditions. According Gao et al., all postmachining files are compatible with GT and GT Series X (Dentsply) rotary file
heat-treated instruments (gold and blue treated) shows enhanced systems. X7 files are compatible with Vortex, ProFile (Dentsply), K3
flexibility and fatigue resistance.20 WaveOne gold undergoes special (SybronEndo, Orange CA), EndoSequence (Brasseler USA, Savannah
heat treatment before and after machining process. Superelastic GA), TF (SybronEndo), and other similar 0.04/0.06 taper rotary file
NiTi alloy is subjected to heat treatment under constant strain in a systems. According to Hansen, X7 files had shown extreme strength
temperature range of about 410–440°C. After griding the working and flexibility on torsion and bending test.25
portion of the file, the finished instrument is heat treated a second Examples: FlexiCON™, SmartTrack™, and Neoendo flex files.
time in a range of 120–260°C. The Af temperature of WaveOne gold
is around 40–60°C. It has the advantage that the gold technology
increases the flexibility and strength of the instrument. Torsional
C o n c lu s i o n
resistance of WaveOne Gold is enhanced by the off-centered Evident changes are documented in the metallurgical properties
parallelogram-shaped cross-section design. of NiTi alloys due to thermomechanical heat treatment. Recent
advancements in the manufacturing process of NiTi alloys will
R e c e n t ly I n t r o d u c e d T h e r m o m e c h a n i c a l ly enhance the quality of endodontic treatment by the development
of newer endodontic instruments with superior mechanical
A lt e r e d N i T i F i l e s properties. Postmachining thermomechanical heat treatment will
Max Wire increase durability of the instrument by increasing the flexural/
First endodontic nickel–titanium instrument that combines the cyclic fatigue resistance. Superelasticity and shape memory effect
property of superelasticity and shape memory effect. These of the NiTi instruments will result from phase transformation on
heat treatment, which offered an promising result in enhancement 12. Duerig TW, Bhattacharya K. The influence of the R-phase on the
of fatigue resistance during root canal preparation in complicated superelastic behavior of NiTi. Shap Mem Superelasticity 2015;1:
curved canals. In future, further research has to be needed for heat 153–161. DOI: 10.1007/s40830-015-0013-4.
13. Santos LD, Resende PD, Bahia MG, et al. Effects of R-phase on
treatment of retreatment file systems and to improve the efficiency,
mechanical responses of a nickel-titanium endodontic instrument:
safety, and quality of endodontic instruments. structural characterization and finite element analysis. Sci World J
2016;2016:7617493. DOI: 10.1155/2016/7617493.
14. Bouska J, Justman B, Williamson A, et al. Resistance to cyclic fatigue
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