Abstract

Aluminium being a cost efficient and low-density materials which shows remarkable
strengthening when cast with element such as Mg and Sc, thus leading to many studies related
to applications such as automobiles, machinery, and aerospace, etc. The aim of this work is to
study the microstructural properties of different Al alloys such as, As cast Al 2021, cast Al-
6.8%Sc, cast Al-5Mg-0.25Sc, Squeeze Cast Al-Mg-Sc alloy and the cold rolled squeeze cast
Al-Mg-Sc alloy. The study was carried out to investigate the effect of different elements of
different composition on its microstructure which in turn effects its mechanical properties such
as strength, hardness, toughness etc.
Therefore, this paper studies the effect of Sc on the Al-Mg alloys produced by the conventional
gravity casting method and squeeze casting method by studying their microstructural properties
of samples such as, As cast pure commercially available aluminium alloy, Al- 6.8%Sc, Al-
5Mg- 0.25Sc which are cast using conventional gravity casting method, and Squeeze cast Al-
Mg-Sc alloy and rolled Squeeze cast Al-Mg-Sc alloy, and differentiates the effect of addition
of Sc element and that of squeeze cast and conventional gravity cast on the alloys
microstructural properties. It is expected to provide a theoretical basis for the optimal design
for the production of high strength and tough 5xxx series cast aluminium alloy composition.

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 Chapter 1: Introduction
1.1 Aluminium and its Alloys
Aluminium is one of the most used metals in the manufacturing industry’s such as aerospace,
Shipbuilding, automotive and machinery’s etc, because of its excellent strength to weight ratio
and for being incredibly light. Aluminium is an element whose mechanical and physical
property can be altered by combining it with other elements such as magnesium, silicon,
scandium, copper, zinc and manganese etc, thus creating the Aluminium alloys with special
properties suitable for required sectors. Aluminium can provide particular required properties
by combining it with other particular elements in a precise ratio for required applications. For
example, when combining aluminium with magnesium forms an alloy which is strong but light
which is perfect in the automotive and aerospace industries. An extensive range of products
such as vehicles, aircrafts, ships and machines etc are composed of aluminium alloys mainly
because of its wide range of sectors due to its low density, corrosion resistance, and thermal
conductivity.
1.1.1 Characteristics of Aluminium Alloy
• High Strength-to-Weight Ratio: aluminium alloys are mainly useful in variety of
applications where the balance between strength and weight must be maintained
carefully because of their low mass and mainly due to their high strength to weight
ratio.
• Corrosion resistance: a protective oxide layer is formed on the surface of the
aluminium alloys whenever they are exposed to air, which enhances its corrosion
resistance properties.
• Lightweight: Aluminium alloys being lightweight element and having low density,
approximately one third of that of steel, making it a much more preferable solution for
situation where weight reduction is very much crucial such as aerospace industries.
• Formability: aluminium alloys are versatile in industrial processes because of their
good ductility which allows for complex designs and intricate detailing. Thus, making
it an easily shaped through processes like extrusion, rolling and forging etc.
• Recyclability: Aluminium alloys are highly recyclable, and the recycling process
requires significantly less energy compared to primary production. Thus, making them
a sustainable choice.

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1.1.2 Different Types of Aluminium Alloy.
Based on their chemical makeup, that is on which element is added to the aluminium alloys
which categorises them to their different series. Thus helping in altering their chemical and
physical properties to any requirement. Those types are listed as:
• 1xxx series
The composition of the 1xxx series alloys is primarily aluminium (at least 99%), with trace
amounts of other metals. They are very ductile, resistant to corrosion, and highly thermally
conductive. Chemical tanks, conductive bus bars, and rivets are just a few examples of goods
that use pure aluminium. What sets apart the various alloys in the 1xxx series from one another
is their exact composition and impurity content.
• 2xxx Series (Copper)
The strength deduced in the 2xxx series of aluminium alloys is mainly due to presence of
copper as an alloying element. These alloys find their applications in different high-
performance industries such as military and aerospace due to their preferable properties such
as high temperature resistance, heat treatment process and machinability etc. The copper
concentration and other trace components differ throughout the alloys of the 2xxx series.
• 3xxx Series (Manganese)
The main alloying element in Aluminium alloys which forms the 3xxx family is manganese,
which enhances the formability and resistance to corrosion of the metal. With their mild
strength, these alloys cannot be heat-treated. They are used in building supplies, automobile
parts, and cookware. They function effectively during anodizing and welding as well.
• 4xxx Series (Silicon)
The primary alloying ingredient in this series is the element silicon which gives Aluminium
exceptional liquid fluidity and very little solidification shrinkage. It has a very good resistance
towards corrosion, but moderately strong, but has good machinability. It is typically utilized in
the automobile industry for engine blocks and other components that require effective heat
dissipation.
• 5xxx Series (Magnesium)
Magnesium being the primary alloying ingredient in the 5 xxx aluminium alloy series, they are
renowned for having exponential resistance towards corrosion, especially in maritime settings.
The primary alloying ingredient being magnesium, offers heat treatment-free moderate to high
strength. The alloys in the 5xxx series are ideal for use in boats, ships, and offshore platforms
because of their superior corrosion resistance, particularly in maritime settings. They retain a

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good deal of their strength even after being easily welded. In addition, hardware, signage,
architectural applications, and other items needing corrosion resistance use the alloys from the
5xxx family.
• 6xxx Series (Magnesium and Silicon)
A propositional mixture of elements of silicon and magnesium in the aluminium alloys, act as
their primary alloying elements in the 6xxx series. They are application lies in the structural
parts such as construction, automotive, and aerospace sectors, due to their machinability, show
of good strength, and due to a notable resistance towards air corrosion.
• 7xxx Series (Zinc)
The 7xxx series of Aluminium alloys is a group in which any other elements are added to obtain
a desired property. Zinc makes up the majority of this heat-treatable alloy, with lower amounts
of copper, magnesium, and other metals. It is very durable, strong, and has outstanding fatigue
resistance and also has a great corrosion resistance. The alloys find application in high-
performance sporting products in aircraft and aerospace. This variety can be welded, although
caution must be used to prevent cracking.
1.2 Casting
Casting is one of the fundamental manufacturing process in which the molten metal is poured
into a cavity known as moulds for the production of solid objects of desired shape, size and
structure, and also for the production of complex components for intricate design and precise
dimensions. Various industries such as automotive, aerospace and constructions widely use
this method for production due to its versatility and cost effectiveness.

Figure 1.1: A basic Schematic representation of casting processes.

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1.2.1 Different Types of Casting.
• Sand Casting
Sand casting has been an essential method for producing metal parts with wide range going up
to tons, it has become a versatile metal casting technique which uses a non-reusable sand
moulds for producing metal parts with intricate design and dimensions. This method has
become an indispensable part of production in different industries due to its excellence in
shaping alloys with high melting temperature such as, steel, nickel, titanium etc. Silica is the
most preferable casting sand while green sand is also used in the production, sometimes
inexpensive and recyclable materials are also combined to make moulding sands with
exceptional heat resistance. Characteristics like strength, permeability and flow ability is
proportional to the effectiveness of the mould in maintaining its shape and producing high
quality casting materials.
• Die Casting (Metal Die Casting)
Die casting or metal die casting is a production method that focuses on precision casting, its
methods mainly involve melting the metals with low melting points and then injecting them
into a long-life die-casting mould. Die casting has become an indispensable part of the modern
manufacturing process used in industries such as automotive, aerospace shipbuilding, and
construction. A high level of accuracy, precision, and repeatability is guaranteed when creating
metal components because of these steel mould being created using cutting-edge techniques
like CNC machining. Die casting has been divided into two separate procedures mainly hot
chamber and cold chamber die casting. Based on their different melting points each process
handles different materials. For example, aluminium is cast using mainly cold casting method
while alloys like zinc, tin, lead, and magnesium are cast using hot chamber casting.
• Investment Casting
Investment casting is a kind of painstaking process in which the ceramic moulds are created
around wax designs to act as an encasement for the molten metals. Multiple wax pattern can
be melted into the system by using a gate system. To create a multilayer casting the pattern is
latter submerged into a slurry or sand. When the wax is removed the melted molten metal is
poured in to create incredibly detailed product. Melted metals such as aluminium or stainless
steel etc are poured to create incredibly detailed reproduction when the wax is removed. Fine
details and smooth finishes are a few benefits that come when using investment casting to
effectively construct complex parts that are challenging to fabricate using other methods.

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Investment casting has become a vital process utilized in numerous industries, protecting good
workmanship and facilitating efficient large-scale production.
• Gravity Die Casting
Melted metal is injected into a mould’s chamber using gravity in the tried-and-true gravity die
casting technique. With its origins in antiquity, this method combines economy and simplicity.
This process can be performed both manually as well as mechanically were in both, the metal
is melted, poured into the cavity, and then the manufacturers wait for the metal to solidify.
Better finishing, reduced expenses and positive mechanical qualities are few of the many
benefits of this process, its main disadvantage can be mentioned as the time it takes to create
complex parts. This technique even with modern improvement works well for smaller parts by
finding applications in kitchenware’s, lights and automobiles, among other areas, while sand
casting and die casting are better suited for intricate and large-scale productions.
• Continuous Casting
Melted metal in a vertical or horizontal mould is rapidly cooled to produce consistent, finely
grained, solid shapes with outstanding physical qualities through continuous casting. This
method leverages gravity to maintain a steady flow, minimizing pollutants while optimizing
the yield. Solids and tubes being the most common shapes, other shapes such as squares
hexagons can also be created. Once the metal is cooled and achieved a required length after
pouring into the mould it is withdrawn consistently. Continuous casting excels when it comes
to producing high density, pressure resistant products for applications which demands
dimensional accuracy and structural integrity. Although continuous casting offers advantages
such as efficient stock use and dimensional consistency, given its expenses and appropriateness
for certain alloys and volumes are considerably disadvantages.
• Shell Moulding
As a part of the precision casting process known as shell moulding a thin mould is made around
a heated metal pattern. A combination of thermosetting resin and dye silica sand forms a shell
of thickness of about 6mm around the pattern. A cavity for pouring the molten metal is created
by joining the dried and stripped shells. Shell moulding is considered as the best option for
mass production of thin-walled casting because it can offer a great dimensional accuracy and
a superior surface finish. It generates patterns with high quality results that guarantee intricate
details and reliable results despite being more expensive comparatively to other methods such
as sand casting.

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 • Lost-Foam Casting
In this casting process, the molten metal is poured to a mould made of foam that evaporates
during pouring, which is encased by sand. The mould made is carved, machined or injected
polystyrene foam. The ceramic refractory coating done is made permeable to a certain degree
so that the waste gas can escape into the sand. The lost-form casting process allows for complex
shapes and thin walls at a lower cost and with less lead time and machining requirements than
many other casting methods. Complex CAD designs and constrained part sizes, however,
present difficulties. This process is used by a variety of industries, including: the arts, defence,
and automotive, to produce a wide range of parts, including circuit boards, sculptures, and
automobile components.
• Pressure Die Casting
High pressure die casting being a modern metal processing method involves rapidly pouring
the molten metal into the mould to produce casting. This process is mainly used because it
boosts strong mechanical properties, minimal machining, high production efficiency and
excellent surface finish. Time, temperature, speed and pressure are the parameters to be
maintained and the compactness of the material is mainly dependent on the filling capacity and
specific pressure. Few examples of pressure die casting include manufacturing of toys,
appliance and automotive housing etc.
• Centrifugal Casting
Concrete, glass, and metal can all be shaped into thin-walled cylinders using the centrifugal
casting technique, sometimes known as rotor casting. It pours molten material into a permanent
mould and swiftly rotates it to create a fine-grained casting with rotational symmetry. The
centrifugal casting method is frequently used to create standardized stock materials for
additional machining rather than generating custom-shaped pieces. Alfred Krupp invented it in
1852, and it's used to build cylinder liners, flywheels, and pipes, among other things.
• Permanent Mould Casting
This method of metal casting helps in the production of accurate, high-quality cast using
reusable moulds which are made of steel or iron. Industrial sectors such as automotive,
aerospace which demands complex shape, superior mechanical properties and production in
large volumes preferably use this method, due its advantages such as its intricate design, fine
grain structure, cost efficiency and smooth finish etc. At the same time its initial installation
cost and problems faced while heat transfer and lack of material compatibility are some of its

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disadvantages. Some of its Innovations mentioned are hybrid processes and CAD and 3D
printing for making moulds.
• Vacuum Casting
Silicone moulds are used in vacuum casting, sometimes referred to as polyurethane casting or
urethane casting, to create rubber and plastic components. This versatile technique imitates
injection moulding to produce castings devoid of bubbles and with flat surfaces. Its application
is most advantageous in low-volume manufacture of complex parts and rapid prototyping.
Vacuum casting is a technique that has applications in the automotive, aerospace, and product
design verification industries. It comes with a wide range of resin alternatives. The flexibility
and cost-effectiveness of vacuum casting are advantageous; however, mould wear and
shrinkage rate must be considered. Innovations include things like additive manufacturing and
the capacity to create complex features.
• Low-Pressure Casting
Low-pressure die casting (LPDC) is a metal die casting process in which molten metal is
poured into a mould at low pressure, typically 20 to 100 kPa. Volume shrinkage during the
solidification process can be controlled using this method by continuously filling the die cavity
maintaining its accuracy. This process produces a comparatively pure samples due to less
oxidation and slag formation. Intricate geometrical design with smooth surface, sharp contours
can be produced by this method. It has limitations in the production of thin-walled parts and
slower cycle times, despite its benefits in accuracy and formability. Automotive parts like
cylinder heads, blocks, and wheels, as well as everyday kitchen appliances like pressure
cookers, are just a few examples of the many applications in which LPDC can be used.
• Squeeze Die Casting
High pressure is used in squeeze die casting, a hybrid of casting and forging, to solidify molten
metal in the space between hydraulic press plates. It yields extremely dense, virtually pore-free
casting in the shape of a net. Each of the two main categories—direct and indirect—has
particular benefits. While direct casting entails pouring metal into a die and pressing it under
pressure, indirect casting is more akin to high-pressure die casting. Better metallic qualities,
faster manufacturing cycles, and enhanced mechanical qualities are the outcomes of the
method. While there are many options for materials, copper, magnesium, and Aluminium are
frequently selected. Squeeze casting is used in a variety of products, including aircraft and
automobile parts.

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1.2.2 Advantages of Casting
• Ability to produce complex shapes easily.
• Versatility—a wide variety of metals and other materials can be cast.
• Cost-effectiveness, especially for small quantities.
• Capability to produce large-sized castings up to 200 tons.
• Cost and time savings compared to other manufacturing methods.
• Suitable for materials that cannot be mechanically worked.
• Simplifies the production of large and heavy components.
1.2.3 Disadvantages of Casting?
• The surface finish may require additional finishing operations.
• Limited mechanical properties compared to wrought materials.
• The possible presence of casting defects like porosity.
• Shrinkage occurring during solidification process sometimes compromise dimensional
accuracy of the cast material.
• Initial equipment installation cost and tooling for some casting method are high.
• Casting is typically restricted for metals having low melting point.

1.3 Gravity die casting

A crucial manufacturing method that is widely used in contemporary industry is gravity die
casting, a kind of permanent mould casting. Using this process, molten metal is poured into a
reusable mould to create intricate metal components. Reducing porosity and air entrapment
during casting is one of the main advantages of gravity die casting. As a consequence, the
components have increased structural integrity and a lower chance of faults.

1.3.1 Advantages of Gravity Die Casting

• Generates high-quality non-ferrous castings characterized by a smooth surface finish
and good dimensional precision.
• Consistently yields non-ferrous castings of good quality. Part-to- part dimensional
stability due to the use of durable steel moulds.
• It is a cost efficient process for manufacturing non-ferrous materials even on large scale.
While the initial investment in tooling and equipment might appear high compared to
sand casting, the cost per part diminishes as production volumes rise.

9
 • Results in less scrap compared to other casting methods, owing to its ability to create
non-ferrous castings with minimal defects and porosity.
• Can work with an extensive array of materials, encompassing such non-ferrous
materials as aluminium, brass, bronze, zinc, magnesium, and copper, among others.

1.3.2 Disadvantages of Gravity Die Casting

• Has distinct requirements that impose limitations on design flexibility. Unlike LPDC
and HPDC which uses high pressure externally for filling up the mould, this process
solely depends on the gravitational force for the molten metal to flow down the moulds.
Achieving specific design features, like thin walls and intricate geometries, can be
challenging within the confines of this method.
• Necessitates a moderately high initial investment in terms of tooling and equipment but
this is comparatively much lower than that of pressure die casting, but at the same time
higher than that of sand casting.
• In comparison to alternative casting methods, gravity die casting typically involves
longer lead times because the fabrication of permanent moulds can take several
months.
• Is most suitable for producing relatively small aluminium castings. The method is less
appropriate for manufacturing larger components. This is because, at the largest sizes,
the permanent mould approach becomes "uneconomical."

1.4 Squeeze casting

Squeeze casting, is a distinctive mixture of process such as casting and forging, helping in the
transformation of metal components manufacturing process. Molten metal gets pumped into a
prepared mould while the machine exerts pressure to guarantee complete filling and accurate
shape. This procedure has become a significant part for producing material with high strength
and intrinsic shape and design. By understanding the importance of control over variables like
temperature and pressure, products with best outcomes can be produced.
Applications of squeeze casting comes under aerospace components and automotive which
require complex and complicated parts such as engine. Squeeze-cast aluminium alloys, for
example, are used in the aerospace industry due to their lightweight yet durable characteristics.
There are disadvantages to take into account, but squeeze-cast metal is usually less porous and
has better mechanical properties than other types.

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1.4.1 Advantages of Squeeze Casting
• Squeeze-cast parts can be heat-treated to enhance their mechanical properties.
• The process offers consistent and reproducible results.
• Squeeze casting helps in the production of components with high mechanical
properties, high strength and ductility etc.
• It helps in producing material with high density and also reduce porosity in them.
1.4.2 Disadvantages of Squeeze Casting
• It can be expensive due to its specialized equipment and tooling requirements.
• Squeeze-cast parts requires substantial machining for obtaining precise tolerances.
• Comparing with other casting process it is a less flexible for complex shapes.

1.5 Aim and Objective

This paper studies the effect of Sc on the Al-Mg alloys produced by the conventional gravity
casting method and squeeze casting method by studying their microstructural properties of
samples such as, As cast pure commercially available aluminium alloy, Al- 6.8%Sc, Al- 5Mg-
0.25Sc which are cast using conventional gravity casting method, and Squeeze cast Al-Mg-Sc
alloy and rolled Squeeze cast Al-Mg-Sc alloy, and differentiates the effect of addition of Sc
element and that of squeeze cast and conventional gravity cast on the alloys microstructural
properties. It is expected to provide a theoretical basis for the optimal design for the production
of high strength and tough 5xxx series cast aluminium alloy composition.

11
 Chapter 2: Literature Review
2.1 Literature on Aluminium and its alloys
Aluminium is a lightweight, corrosion-resistant, and highly conductive metal used extensively
across various industries. Aluminium alloys are produced by combining aluminium with other
elements such as copper, magnesium, manganese, and zinc, which enhances its strength,
hardness, and other properties.
The primary types of aluminium alloys include:
• 1xxx series: Super-pure and commercial-purity aluminium
• 2xxx series: Aluminium-copper and aluminium-copper-magnesium alloys
• 3xxx series: Aluminium-manganese and aluminium-manganese-magnesium alloys
• 5xxx series: Aluminium-magnesium alloys
• 6xxx series: Aluminium-magnesium-silicon alloys
• 7xxx series: Aluminium-zinc-magnesium and aluminium-zinc-magnesium-copper
alloys
2.1.1 Benefits of Aluminium Alloy
• Low Density: When weight reduction is essential, aluminium alloys are ideal. Things
made of aluminium weigh far less than those made of other metals.
• Excellent Strength-to-Weight Ratio: For a given density, aluminium alloys have a
higher strength than many other materials.
• Corrosion Resistance: Due to their superior corrosion resistance, aluminium alloys are
ideal for usage in abrasive conditions, such as industrial or maritime settings.
• Ductility: The majority of alloys made of aluminium are quite ductile, making forming
easier and free from cracking or breaking.
• Thermal Conductivity: Aluminium alloys are excellent thermal conductors in any area
where effective heat transfer is required.
2.1.2 Limitations of Aluminium Alloy
• Lower Melting Point: Aluminium alloys may not be the best choice for high-
temperature applications because their melting point is lower than that of the majority
of other structural metals.
• Lower Hardness: Due to its relative softness, aluminium is less durable than some
other materials.
• Higher Cost: Compared to other materials, aluminium alloys cannot be as economical
in some applications.

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2.2 Literature on Al-Mg-Sc alloy
An Al-Mg-Sc alloy is a type of aluminium alloy in which magnesium (Mg) and scandium (Sc)
serve as the primary alloying components. In Al-Mg-Sc alloys, aluminium is often the base
metal, to which small quantities of scandium and magnesium are added. Extremely small
amounts of scandium—typically less than 1%—are added to the alloy to improve its properties.
Common processes for fabricating aluminium alloys, including casting, forging, and
machining, can be applied to Al-Mg-Sc alloys. It could be necessary to modify the processing
parameters after adding scandium in order to maximize its properties.
The urgent demand for large, complex, high-strength, corrosion resistant and tough aluminium
alloy structural parts for the high-end manufacturing fields such as aerospace, shipbuilding, rail
transit, national defence, and military industry have significantly increased in the past few
decades. Considerable endeavours have been made to develop high strength, corrosion
resistance and toughness aluminium alloys that can be directly cast into structural components
[1-6]. To overcome the poor castability of high strength and toughness aluminium alloy,
various techniques have emerged, such as powder metallurgy, rapid solidification processes,
electromagnetic casting processes, and so on [7-9]. But due to their complexity and higher cost
rate these techniques have been commercially avoided. On the other hand, squeeze casting as
emerged as a promising technique, which leads to a better microstructural and mechanical
properties of cast components that can be compared to those of conventionally cast
components, sometimes even close to that of forged counterparts [10,11].
Strong and durable aluminium alloys also show high levels of alloying, a wide range of
solidification temperatures, significant solidification shrinkage, a high propensity for alloy hot
cracking, poor casting performance, and extreme difficulty in direct casting moulding [12].
Rough grains and segregation are also present in the castings [13]. It is challenging for the
material's mechanical characteristics to approach those of a deformed aluminium alloy due to
these issues. Thus, it has become crucial to conduct research and development on Al-Mg-Sc, a
high-strength, corrosion resistance and tough cast aluminium alloy with good mechanical and
casting properties, in order to meet the pressing demand for low-cost, Corrosion resistant,
lightweight key structural components for the aerospace, shipbuilding, rail transit, national
defence, and military industries, as well as to realize equipment upgrading [14-16].
Even though the Al-Mg system alloys has good fluidity, the porosity of the material also
increases due to air getting trapped inside the mould during the poring process in conventional
gravity casting, thus the pressure used in squeeze casting is sufficient to drive the melt into the
mould cavities such that no air particles are trapped inside. This can help in simultaneously
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boosting the strength and toughness of the alloy while also help in significantly decreasing the
porosity of the casts [17-20]. Additionally, the pressure can decrease intergranular segregation
and also improve the solubility of solute atoms [21, 22]. By adding certain transitional and rare
earth family elements to aluminium alloy is another way to enhance aluminium alloy castability
and its mechanical characteristics [23, 24]. These elements serve two purposes: first, they
increase melt fluidity and shorten the solidification range; second, they interact with Al or Mg
atoms to form intermetallic compounds (IMCs) with high melting points that enhance high-
temperature mechanical properties [25]. Moreover, these elements have the ability to accelerate
or slow down precipitated phase growth rate [26-29].
Since 5xxx series aluminium alloys have relatively few eutectic components that have a feeding
effect during solidification, it is difficult to flow when blocked by dendrites, and hot tearing is
easily generated. The smaller the grain size of the alloy, the better the fluidity of the alloy, and
better the shrinkage during cooling and solidification which in turn helps in improving tensile
strength and ductility of alloy. By controlling the solidification conditions, a fine grain structure
can be obtained by increasing the number of crystal nucleation cores while suppressing grain
growth. Therefore, adding a refiner to the melt can effectively refine the grain structure of the
alloy [30], which is considered the simplest and most effective method. Sc and Zr elements are
commonly used grain refiners in 5xxx series of aluminium alloys [31–35], as they promote the
refinement and homogenization of the grain size in the Aluminium alloy, as well as help them
in reducing the segregation and hot tearing sensitivity of the alloys.
The clustered atomic groups in the melt of the aluminium alloy interact with the Zr elements
to generate atomic clusters when a small amount of Zr is added to the melt. Eventually, these
atomic clusters grow into the nucleation core of newly formed grains. The peritectic reaction
will occur in the aluminium alloy as the Zr element content increases and become the core of
the equilibrium grains, preventing the growth of grains and segregating them even more.
However, the impact of crystal grain refinement in the real non-equilibrium solidification
process is restricted, and the solubility of Zr element in the melt is comparatively less than that
of Sc. According to the studies of Dev [36], commercial aluminium alloys can achieve a non-
dendritic structure and much finer grain structure by adding 0.1% of Zr and at least 0.18% of
Sc. A detailed Al3(Sc, Zr) phase is formed when Sc and Zr are added to aluminium alloys [37-
39]. For the significant grain refining effect to be observed, the content of the Sc element alone
must be greater than 0.55%. But when the compound is introduced during the actual production
process, the total amount of Sc and Zr added is often less than 0.3%, which can accomplish the
evident refining effect while also minimizing costs. Although many studies have been carried
14
out on the microstructure and properties of 5xxx aluminium alloys series by adding Sc and Zr,
there is no report on the effects of adding Sc on the casting properties of new high-strength,
tough and corrosion resistant cast aluminium alloys with a high Mg ratio.

Table 2.1: Yeild strength and Elongation of different composition and different methodology
studied in different papers.
Sl Reference Composition Casting YS Elongation
No paper no. methodology
1 1 Al-Zn-Mg- Conventional 552 MPa 11%
Cu casting method
2 1 Al-Zn-Mg- Rheo-Squeeze 571 MP 14%
Cu casting method
3 2 wrought Rheo-formed 483 MPa 8%
7075 samples in the T6
aluminium condition
alloy
4 6 Al-5Cu- Squeeze cast 348 MPa 16.5%
1Mn-1Ni
alloy
5 9 TiH2- additive 485 ± 41 MPa 10.0% ± 2.5%
modified Al- manufacturing
Zn-Mg-Cu
alloy
6 15 Al–Zn–Mg– e pre-annealing + 12.0% -13.3%
Cu alloy T6 treatment
(7A04 alloy)
7 21 AA2024 squeeze casting 340 MPa
aluminium
alloy
8 22 7075 Al squeeze casting 345.5 MPa 7.6%
alloy

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9 25 Al–6Zn– Squeeze 605.67+32.22% 8.1%+15.71%
2.5Mg– casting+ solid hot
1.8Cu alloy extrusion
10 28 Al-5.0Cu- squeeze casting+ 330 MPa 18%
0.4Mn alloy T6 heat treatment

11 29 Al-7.6Zn-1.6 permanent mould 647 MPa 6.8 %

Mg-2.1Cu casting
(wt.%) alloy method+T6 heat
Treatment
12 31 Al-Zn-Mg- Gravity Cast + 721 MPa 10.9%
Cu-Sc-Zr homogenizing,
alloy hot-extruding,
then solid-
solution and aging
(T6)
13 34 Al–Zn–Mg– Cast + rolling, 627 MPa 11.5%.
Sc–Zr alloys annealing and
aging processes
14 36 Al-Zn-Mg- spray deposition 684 MPa 17.4%
Cu-Zr alloys
15 40 Al-Zn-Mg- permanent mould 647 MPa 6.8%
Cu-Zr-Ti-Y casting method
alloy with
low Zn and
Mg content
16 41 aluminium squeeze cast 172.5 MPa
alloy
A380+Ni+Sr
17 42 Al-Mg- Laser Powder Bed 475 MPa 8.5%
0.7Sc-1.0Ti Fusion
alloy

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2.3 Casting
Casting is a manufacturing process in which the material is heated to its melting point and the
molten material, like metal, is poured into a mould and allowed to harden. To retrieve the cast
once solidified the mould is broken. This process helps in producing intricate complex
components with specific properties.
2.3.1 Importance of Casting in Manufacturing
The importance of casting in manufacturing process is that it helps for the production of
intricate, complex metal components more cost-effectively. As casting can produce multiple
pieces in a single unit it greatly decreases the number of individual parts needed. This reduces
the overall cost and also simplifies the streamlines inventory management and assembly
processes. Casting helps in enhancing the efficiency and productivity of materials by reducing
the need for excess welding and joining.
Table 2.2: Different Casting methods and their respective properties.
Casting Process Metals Tolerance Surface finish Min thickness
(RMS)

Gravity Die Cu, Al, Zn, Standard +/- 0.015" to 150 -300 0.188"
Casting and cast 1" then add +/- 0.002"
irons / inch
Sand Casting All Metals Standard +/- 0.030" up 500-2000 0.150"
to 6", Add +/- 0.002"
for every inch over 6
Low-Pressure Al, Cu, Zn, Standard +/- 0.015" to 150 -300 0.188"
Die Casting Mg 1" then add +/- 0.002"
/ inch
High-Pressure Al, Zn, and Standard +/- 0.010" to 32-63 (Zinc); 63- 0.030"(Mg) to
Die Casting Mg 1" then add +/- 0.001" 250 (Aluminium) 0.060"
/ inch (Aluminium)
Investment Al and Standard +/- 0.005" to 63-250 0.060"
Casting (lost Steel 3" then add +/- 0.003"
wax casting) / inch

17
 Squeeze Al Standard +/- 0.010" to 90-500 0.30"
Casting: 1" then add +/- 0.001"
/ inch
The integration of advanced technologies holds a significant effect on future casting
methodology. Optical measuring systems, such as the ATOS 3D Digitizer, are revolutionizing
the industry by enabling efficient and accurate measurement of complex surfaces. These
systems eliminate the laborious and time-consuming nature of traditional measuring methods,
providing full-field measurements and faster validation. Embracing such technological
advancements will enhance productivity, quality control, and overall efficiency in the casting
process. In this work two of the most used casting methods was used in the production of the
samples and they were the gravity casting method and the squeeze casting method. These
methods were chosen because of their vast castability, productivity and reusable conditions.

2.4 Gravity Die Casting

Gravity die casting is a manufacturing process used to produce high-quality metal parts with
complex shapes and relatively smooth surfaces. It's a type of casting method that falls under
the broader category of die casting processes. The key characteristics differentiating gravity
die casting from other casting methods are that (1) only the force of gravity is used to introduce
the casting metal into the mould; and (2) a reusable ("permanent") metal mould is used. It is
usually made of steel or cast iron.
2.4.1 Limitations of gravity die casting.
• Limited design flexibility: In order to facilitate the flow of molten metal under gravity,
gravity casting necessitates certain design considerations. It could be challenging to
create thin walls and complex geometries.
• High initial cost: Gravity casting necessitates a large tool and equipment upfront cost,
which may be prohibitive for new or small enterprises. Low-volume production may
also be concerned about the cost of tooling.
• Longer lead times: The time needed to create the mould, which can take several weeks,
makes gravity casting generally have longer lead times than other casting techniques.
• Limited part size: The production of comparatively small parts is the ideal application
for gravity casting. Large pieces are not a good fit for this procedure because the weight
of the molten metal can warp or shatter the mould.

18
 • Restricted material properties: The uniform grain structure that gravity casting
creates in parts may limit the part's strength and toughness. Stainless steel is one
material that could not be appropriate for gravity casting.

2.5 Squeeze Casting

Squeeze casting is a manufacturing technique that combines casting and forging. It’s also
known as liquid metal forging. This technique involves injecting molten metal into a heated
die, allowing it to begin solidifying, and then closing the upper die to form the mould chamber.
Pressure from the upper die forces metal to completely fill the casting cavities which results in
outstanding surface quality and minimal shrinkage. Aluminium and magnesium alloys are the
most common metals for this procedure, but it can accept others as well. Vehicle parts are very
often squeeze-cast.
2.5.1 Types of Squeeze Casting.
• Indirect Squeeze Casting
In indirect squeeze casting, molten metal is introduced into a shot sleeve. This is then forced
through relatively large gates into the die cavity at low velocity (usually less than 0.5 m/s).
High pressure is applied "indirectly" through the extensive gating system. This process controls
solidification, so it prevents defects, but the gating complexity increases material and energy
use.
• Direct Squeeze Casting
Direct squeeze casting (DSC) involves pouring liquid metal into a heated, lubricated die and
forging it as it solidifies. Pressure is applied shortly after the metal begins to freeze and is
maintained until the entire casting has solidified. DSC is commonly executed using a vertical
apparatus that resembles a forging press in its operation.

2.5.2 Applications of Squeeze Casting

Many industries use squeeze casting to create complicated, high-quality metal components. A
few examples are found in the production of: steel bevel gears for machinery, aluminium domes
for architectural use, iron mortar shells, pistons for internal combustion engines, aluminium
automotive wheels, and bronze and brass gear blanks. This procedure guarantees superior
mechanical qualities and dimensional accuracy in these components.

19
2.5.3 Advantages of Squeeze Casting
• Squeeze-cast parts can be heat-treated to enhance their mechanical properties.
• The process offers consistent and reproducible results.
• Squeeze casting yields components with excellent mechanical properties, including
strength and ductility.
• Squeeze casting results in low porosity, ensuring high-density components.
2.5.4 Disadvantages of Squeeze Casting
• It can be expensive due to its specialized equipment and tooling requirements.
• Squeeze-cast parts may require extensive machining to achieve precise tolerances.
• It is less versatile for complex shapes compared to other casting methods.

20
 Chapter 3: Experimental procedure
3.1 Electric resistance furnace
The Aluminium alloys of compositions mentioned in Table 3.1 were fabricated by using the
electric resistance furnace. Figure 3.1 shows the standard setup of an electric resistance furnace
that was used. As per the size of furnace’s crucible, the total material to be melted was taken
as 100 grams each time. The crucible is filled with the metal that is to be melted, and an
additional device is fitted to the furnace for addition of excess material or other elements for
complex compounds. The heating material inside the furnace consists of high resistance
material such as kanthal or nichrome, because of their high-resistance when current flows
through them large amount of heat is produced. The furnace’s interior is lined or coated with
refractory materials to prevent any heat loss and to tolerate high temperatures.
Once the furnace is charged electric energy is supplied to the heating element. Heat is
transferred to the crucible made of graphite, which is used because of its high stability at high
temperatures, good thermal conductivity, and ability to transfer heat. Thus, helping in the
process of melting the material inside the crucible at the desired rate and proposition. To ensure
effective melting without overheating the furnace, operators can modify the power supply to
maintain the desired temperature, with the help of thermocouples fitted to the furnace. The
aluminium starts to liquefy as the temperature inside the furnace starts to rise to its melting
point, the temperature is regulated so that the quality of the material is regulated and impurities
can be eliminated. The completely melted material is poured into the mould for casting, for this
reason, the crucible can be removed from the furnace easily thanks to its design.

(a) (b)

Figure 3.1: (a) gives the electric resistance furnace used for melting and (b) gives the
conventional furnace used for pre- heat treatment of crucibles.

21
3.2 Sample Preparation
As cast Al-2021, 99% pure Al, 99% pure Sc and 99% pure Mg was taken as the starting raw
materials. Table 3.1 shows the alloy composition for all samples (in wt.% here after),
A= commercial Al-2021, B= Al-6.8Sc, C= Al-Mg-Sc. Metal chunks were weighed according
to the target compositions using a 2000g capacity weighing (Make, DGT-2) scale with a
resolution of 0.01g.
Table 3.1: Alloy compositions (wt.%)
Alloys AA 20221 Al-6.8 Sc Al-Mg-Sc Al-Mg-Sc
Gravity cast Squeeze cast
Sc - 6.8 0.25
Mg 1.3 - 5
Cu 4.4 - - -
Al Bal. Bal. Bal. Bal.

As cast commercially available pure 2021 was taken as the initial sample for the experiment
using conventional gravity casting method. The ingot sample was melted in a graphite crucible
using an electric resistance furnace at temperature around 700°C, and poured into a rectangular
mould for solidification which was preheated at 200°C. The sample was then cut into small
pieces of required dimensions and mounted by cold mounting process and then polished using
Sic wet grinding papers of 120, 220, 400, 600, 800 and 1200 grit size and later polished using
a diamond lubricant- Aerosol DL001 as an abrasive to a 2µm - 4µm surface finish. Later on,
the sample was etched using Keller’s reagent to reveal its grain structure.
The Secondary sample was prepared by melting the pure aluminium ingot which is available
commercially, at a temperature of 700°C and Sc was added to the melt of wt.% 6.8% and stirred
for equal distribution of elements. Later the melt was solidified and a sample for analysis was
prepared using the same methods as for the first sample.
The third sample was prepared in a similar manner with an addition of wt.% of 5% Mg and
0.25% Sc to the pure aluminium ingot melted around 700°C. The solidified sample was
prepared for characterization in a similar pattern as mentioned before.
The fourth sample was obtained from CSIR-NIIST, Thiruvananthapuram, as an Al-Mg-Sc
alloy prepared using the squeeze cast method. The sample was cut to a required dimension and
polished using the same method to obtain a fine surface finish for obtaining some good optical
microstructures.

22
The remaining squeeze cast sample was cold rolled using a four-high-cold-rolling mill to study
the effects of rolling on the microstructure of the sample. The rolled sample was cut into small
pieces to determine the microstructure of RD (Rolling Direction) –TD (Transvers Direction)
and ND (Normal Direction), after polishing and etching using the same process as above.

3.3 SEM and Optical microscope

Microstructural features of the alloys were studied using an optical microscope and later on
using ZEISS EVO 18 scanning electron microscope (SEM) was used to analyse the eutectic Al
alloy in detail in back scattered electron (BSE) mode. A voltage in the range of 15 to 25kV was
used. Energy dispersive X-ray spectrometry (EDS) was done using the same equipment for
elemental identification and approximate composition calculation using the TEAM eZAF
Smart Quant Software.

Figure 3.2: displays the (a) optical microscope and (b) Scanning electron microscope (SEM)
setups used.

3.4 X-ray Diffraction

X-ray Diffraction analysis was done to verify the expected phases in the aluminium and its
alloy system. Sample preparation was similar as mentioned in Section 3.2., where the
specimens were cold mounted and polished till the mirror finish was obtained and then cut and
removed from the mount for analysis. The D8 Advance BRUKER, which is an automated
multipurpose X-ray diffractometer, was used for this purpose along with its DIFFRAC-EVA
software. The identification was done using a standard Cu Kα X-ray radiation source with a
wavelength (λ) of 1.5406 Å and IS 5mm slit. The measurements were run in a continuous mode

23
for different angles and speeds to catch both high and low-intensity peaks. All the samples
were conducted at angles between 10° to 80° at a scan speed of 1°/min. each sample took
around 70 minutes for a complete scan process. The obtained data was analysed using Origin
Pro 2019 software. The peak identification was done by data mining using the databases for
various phases provided by the International Centre for Diffraction Data (ICDD) and the graphs
were plotted with the help of Origin Pro 2019 software.

Figure 3.3: XRD setup used for the analysis.

3.5 Micro-hardness Testing
The main aim of this experiment was to provide an insight into the mechanical properties of
the chosen Al-6.8 Sc, gravity cast Al-Mg-Sc and Squeeze Cast Al-Mg-Sc alloys through a
proxy test. Multiple measurements were taken to rule out any possibility of localized defects
in the samples. This test was conducted in conformance with the procedures listed in the
standard ASTM E384 [30]. The micro-hardness test was done using the Vickers method on a
Wilson VH 1202 Vickers micro-hardness tester. Figure 3.4 shows an overview of standard
setup and sample mounting for testing purposes. This test consists of indenting the sample with
a diamond indenter which has a pyramid shape with a square base and opposite faces at an
angle of 136°. A load of 300 g-f was applied for a dwell time of 10 s on gravity cast Al-6.8Sc
and Al-Mg-Sc alloy, while a load of 500 g-f was applied for the Squeeze cast Al-Mg-Sc sample.
The length of two diagonals on the indent after removal of load were measured using an inbuilt
digital microscope in the test machine and the mean of this was used to calculate the Vickers
hardness number (HV).

24
The presence of scratches on the polished surface do influence the value of Vickers hardness
and thus indentations were induced on surfaces away from any scratches. A minimum of 3
measurements were performed on each sample to minimize error. All experimental error
obtained represent one standard deviation from the mean value.

Figure 3.4: Wilson VH1202 setup used for the analysis

25
 Chapter 4: Results and Discussions
4.1 X ray diffraction:
Figure 4.1 shows the XRD data for a binary eutectic Al3Sc and Al matrix of commercially
available Al 2021 alloy, gravity cast Al-6.8Sc alloy, gravity cast Al-Mg-Sc alloy and Squeeze
cast Al-Mg-Sc alloy. The obtained peaks clearly show the presence of primary Al phase and
minor peaks of Al3Sc phase which is in coordination with microstructural analysis and results
obtained through Thermo-Calc in Xu, Y et al [1]. This pattern matches the ICDD database for
FCC α-Al (00-004-0787) as represented by Figure 4.1 with high intensity peaks at 2𝚹 values
of 38.18°, 44.38°, 64.79° and 77.92° for the Al matrix and 39.21°, 45.45°, 65.76° and 78.89°
for the Al3Sc matrix. A scan was conducted to capture the weak peaks of Al3Sc and confirmed
with ICDD database (04-007-1107 and 00-030-0007) as shown in Figure 4.1.

8x104
(111) Al
7x10 4 Al3Sc
(200) Al 2021
(220) (311)
6x104

(111)
5x104 cast Al-6.8Sc
(111) (200) (220) (311)
(220)
4x104 (200) (311)

(111)
3x104
cast Al-Mg-Sc
Intensity

(111) (200) (220) (220) (311)

(200) (311)
2x104
(111)
Squeeze cast Al-Mg-Sc
1x104 (200)
(220) (311)
0

10 20 30 40 50 60 70 80
2 theta
2θ
Figure 4.1: XRD analysis of Al 2021, binary Al-6.8Sc alloy, treasury Al-Mg-Sc alloy prepared
through gravity casting process and Al-Mg-Sc alloy by Squeeze cast method is
shown respectively from the top as mentioned, at 2𝚹 from 10° - 80° and at a scan
speed - 1°/min.

26
The Al3Sc intermetallic phase has a monoclinic lattice with P21/a space group and lattice
parameters of a: 8.557 Å, b: 6.209 Å, c: 6.213Å, 𝛽 = 94.76°. The obtained XRD peaks agrees
with the characterization done by Xu, Y. Zhang, Z et al [1], H.M. Guo [2], Y.T. Xu et al [3],
T. Liu et al [5], and X.H. Liu et al [9]. The variation in peak intensities for Al3Sc phase is
suggested to be due to preferred orientation of Al3Sc intermetallic [5] as seen in Figure 4.1.

4.2 Microstructural Analysis:

4.2.1 Optical microscopy:
Figure 4.2 presents optical images of studied alloys in the as-cast condition. Figure 4.2(a)
shows the incomplete grain boundaries formed in the Al 2021 alloy. A globular structure is
seen in Figure 4.2(c) for Al-5Mg-0.25Sc indicating the hypoeutectic nature of the alloy and its
inter dendritic structure. The eutectic colonies between these globules are due to the addition
of Mg and Sc elements. The darker lamellar areas as seen depict eutectic Al-Al3Sc, and the
lighter areas show Al matrix. Figure 4.2 (b) resemble an Al-Sc binary system which has a
hypoeutectic structure as well. A mixture of globular morphology with eutectic regions in
between can be seen in this alloy whereas a completely eutectic structure is obtained for Al-
Mg-Sc produced through conventional gravity casting method as shown in Figure 4.2 (c). The
same eutectic composition was concluded for an Al-Mg-Sc alloy produced through Squeeze
cast method as shown in figure 4.2 (d) and (e). The predominant morphology is characterized
by fine, homogeneous, and dense Al3Sc dispersed in the Al matrix figure 4.2 (d) depicts Al
rich zones between the eutectic colonies. This is the result of nucleation of primary Al over
primary intermetallic.
As stated by Garrett et al [26], at high rates of solidification, the nucleation of primary
intermetallic gets suppressed and primary Al nucleates. Z.Q. Han [10], have also discussed this
presence of Al rich zones using the coupled zone concept which states that for higher crystal
growth rates, the primary dendrites (Al matrix) grow along with eutectic colonies. The eutectic
microstructure in Figure 4.2 (c), when observed closely displays a variation in the morphology.
A certain irregularity can also be observed in the eutectic microstructure ranging from fibrous
(rod-like) morphology to discontinuous lamellar structures. Z.Q. Han [10], observed similar
microstructural configuration for an Al-Mg-Sc alloy which was prepared by Squeeze casting.
From Figure 4.2 (d) and (e), it can be observed that the eutectic structure is not continuous and
has small blocky patterns of similar characteristics and directionality. This is again due to the
solidification conditions, as the formation of Al3Sc makes nearby liquid depleted of Sc. From
Figure 4.2 (b) and (c), as compared to Al-6.8Sc, the globules (pro-eutectic Al) in the as cast
27
Al-Mg-Sc become finer and smaller. This depicts the increased percentage of eutectic colonies
at a specified addition of Mg and Sc content rather than a higher addition of Sc content.

Figure 4.2: Representing micrographs of (a) commercially available Al 2021 at 50x, (b) gravity
cast Al-6.8Sc at 50x, (c) gravity cast Al-Mg-Sc at 200x, (d) Squeeze cast Al-Mg-
Sc at 200x and (e) Squeeze cast and rolled Al-Mg-Sc alloy at 200x.

It was determined that the addition of 0.25 % Sc along with 5% Mg by weight provided thinning in the
grain structure in the microstructures. Addition of 6.8% Sc resulted in reduction in dendrite arms. It has
been observed that adding 0.25 % Sc along with 5% Mg by weight has a grain refining effect. As seen
in the microstructures, the silicon length in the eutectic regions has been observed to decrease greatly
due to the scandium addition. The shape was observed to change from needle to spherical shapes with
the addition of scandium, thus exhibiting the well-known phenomenon of modification according to
Cezmi ÖNER et al. Thus addition of Mg and Sc element at an adequate proportion produces a refined
thinner grain structure than simply adding Sc element at a higher proportion.

4.2.2 Grain size distribution:

According to the equivalent circle diameter (ECD) measurements, adding Scandium element
alone did not help contribute to the reduction of grain size. It was observed that the addition of
6.8 wt.% Sc caused an increase in grain size to 38μm on average, compared to the commercial
Al 2021 alloy. While the increase in the amount of Scandium caused significant increases in

28
the grain size, it is also observed that the inter dendritic domain distribution decreases to 34µm
by combining Mg element in alloy produced by conventional gravity casting method. While
the grain size decreases further to around 25µm of the same Al-Mg-Sc alloy produced through
Squeeze casting method. Further it is noted that the average grain size tends to increase slightly
after the cold rolling process due to the combining process of smaller grains with their
surrounding grains under the cold rolling pressure. Figure 4.3 shows macrostructure as well as
their grain size calculated to produce a graph by ECD method of each sample. The general
grain size average is presented in graphs given in order to be easily compared.

Figure 4.3: (a) Average grain size calculated using ECD for the alloy Al-2021.

Figure 4.3: (b) Average grain size calculated using ECD for the alloy Al-6.8Sc, produced
through gravity casting.

29
Figure 4.3: (c) Inter dendritic domain size distribution calculated using ECD for the alloy
Al-5Mg-0.25Sc, prepared by conventional gravity casting method.

Figure 4.3: (d) Average grain size calculated using ECD for the alloy Al-Mg-Sc, prepared by
squeeze casting method.

Figure 4.3: (e) Average grain size calculated using ECD for the alloy Al-Mg-Sc, prepared
through Squeeze casting method and which underwent cold rolling process.

30
One of the factors that increase the strength is the grain size. If this phenomenon is large in a
structure, the strength decreases, if the grain size is small, the strength increases. Smaller grain
structure increases the strength as it will reduce the space between the grains and bring the
grains closer together. However, it was observed that the addition of Sc caused an increase in
grain size compared to the Al-Mg-Sc alloy. Therefore, the addition of only the Sc element did
not show an increase in strength.

4.3 Scanning electron microscopy (SEM)

SEM results are shown in Figure 4.4 gives a clear representation of incomplete grain
boundaries of the Al 2021 alloy prepared. Figure 4.5 And 4.6 gives the micrograph of Al-6.8
Sc and Al-5Mg-0.25Sc respectively which shows a comparatively complete grain boundary.
According to the SEM Micrographs, when the structures were examined, it was concluded that
the amount of porosity increased in direct proportion with the amount of Sc present. In addition,
although it has a ductile structure in terms of fracture behaviour, there are indications of brittle
fracture states. In addition, it was observed in the obtained SEM images that the porosity ratio
increased with the increase in the amount of Sc. While in Figure 4.6 and 4.7 It can be seen that
the addition of Mg along with Sc has reduced the porosity of the sample considerable.

(a) (b)

Figure 4.4: SEM Micrographs of Al 2021 at (a)10µm magnification and (b) 2µm
magnification

31
 (a) (b)

Figure 4.5: SEM Micrographs (a) Al-6.8Sc at 10µm magnification and (b) Al-6.8Sc at 20µm
magnification

(a) (b)

Figure 4.6: SEM Micrographs of gravity cast Al-Mg-Sc at (a) 10µm magnification and (b)
20µm magnification.
From figure 4.7 And figure 4.8 SEM micrograph we can clearly observe the needle like grain
structural formation of sample prepared through Squeeze cast method. It can be observed that
the porosity of the samples is greatly reduced. In the SEM analysis, it was observed that the
grain structure was needle-like. Needle-like structures reduce the strength values. For this
reason, it is desirable that the grains are spherical in structures where high strength values are
desired. It was observed that the addition of scandium element increased the needle-like
structure in the samples examined. In addition, as the amount of Sc increased, it was observed
that the dendrite arms extended. The increase in dendrite arm lengths is directly proportional
to brittleness [33] and the strength of the structure decreases as the dendrite arm length
increases. The addition of scandium did not cause an increase in the strength values, and it was
found that the strength decreased due to the reasons stated [33]. Obviously, if this situation is
associated with the tensile test results, it is also a proof of the increase in material toughness.
However, with the increase in the amount of Sc added, this turns into the results of the reference

32
sample. In other words, the increase in the amount worsens the mechanical properties, which
is an indication of the acquisition of similar images with the reference in SEM images.

(a) (b)

Figure 4.7: SEM Micrographs of Squeeze cast Al-Mg-Sc at 10µm magnification.

(a) (b)

Figure 4.8: SEM Micrographs of Squeeze cast and cold rolled Al-Mg-Sc at 20 µm and 10µm
magnification respectively.

4.4 Energy Dispersive Spectroscopy (EDS)

As shown in the Figure 4.9 when the EDS results were examined, Sc element was found in the
marked region spectrum in the samples containing only 6.8 wt.% Sc. In the spectra taken, it
was observed that the Sc structure was not homogeneously distributed. Details about marked
region spectrum are given in table 4.1 respectively. EDS mapping of Al-Sc with 0.6 wt.% Sc
at 10μm is represented in Figure 4.9.

33
Figure 4.9: Represents the spectrums received when examining EDS results as (a) EDS (Energy
Dispersive Spectrometry (b) Selected area 1 and 2.

Table 4.1: EDS analysis of sample Al-6.8Sc

Elements Graph 1 Graph 2

Wt% Atomic % Wt% Atomic %
Al 88.75 92.93 94.4 95.82
Sc 11.25 7.07 5.6 4.18
Total 100 100 100 100

Figure 4.10: Spectrum received when

examining EDS results as (a) EDS
(energy dispersive spectrometry)
image, (b) selected area 1, (c) selected
area 2, (d) selected area 3.

34
Table 4.2: EDS analysis of sample Al-Mg-Sc by gravity casting method.

Elements Graph 1 Graph 2 Graph 3

Wt% Atomic % Wt% Atomic % Wt% Atomic %
Al 96.47 96.27 95.84 95.62 96.06 95.84
Mg 3.17 3.52 3.72 4.12 3.54 3.92
Sc 0.36 0.21 0.44 0.26 0.40 0.24
Total 100 100 100 100 100 100

Figure 4.11: Represents the spectrums received when examining EDS results as (a) EDS
(Energy Dispersive Spectrometry), (b) Selected area 1, (c)selected area 2
(d)Selected area 3 and (e) EDS spot 1, as noted.

Table 4.3: EDS analysis of sample Al-Mg-Sc by Squeeze casting method.

Elements Graph 1 Graph 2 Graph 3 Graph 4

Wt% Atomic% Wt% Atomic% Wt% Atomic% Wt% Atomic%
Al 60.41 71.77 60.91 72.20 94.83 95.16 83.66 82.60
Mg - - - - 3.58 3.98 15.37 16.84
Sc 39.59 28.23 39.09 27.80 0.52 0.31 0.59 0.35

35
 Others - - - - 1.07 0.55 0.38 0.21
Total 100 100 100 100 100 100 100 100

EDS method was applied to determine the Sc ratios in the structure. As understood from the
EDS results, Sc is not homogeneously distributed in the structure. Therefore, Sc element was
not found in every spectrum taken. The homogeneity of the structure in the casting ensures the
same feature to be seen in all regions on the material. In cases where the structure is not
homogeneous, the same feature cannot be seen in every region on the material. Therefore, the
material is not reliable. A homogeneous structure is desired, especially in structures that are
exposed to high and dynamic strength and corrosion resistive, to show the same feature from
every part of the structure. In general, it has been concluded that the addition of Sc is preferred
to improve the mechanical properties and corrosion resistive of the Aluminium alloy. The
results obtained were compared with other literature studies and it was observed that similar
results were obtained. As an illustration, Xu, Y et al. [1] show that Al-Sc alloys showed
excellent Mechanical properties. In a different investigation, compared to the Sc-free alloy,
cast Al-Mg-Sc containing around 0.2% by weight of Sc was able to increase micro hardness
by approximately 30% and tensile strength by approximately 19%. by Lathabai & Lloyd's [43].
Tzeng Y.-C. et al. [44] shows that 0.25 wt.% scandium has the potential to improve tensile
strength by ~27%. They also found that the improvement of ~13% and ~14% in the Vickers’s
hardness and Charpy impact strength, respectively with 0.3 wt.% Sc addition to the alloy. S.L.
Pramod et al. [12] investigated the wear and hardness of Al alloy with Sc. They showed with
0.4 wt.% Sc alloy and 0.4 wt.% Sc–10 wt.% composite hardness of the material increases up
to 20% respectively. Another study done by S.L. Pramod et al. [12] in tensile test of Sc to Al
indicates that the addition of 0.4 wt.% Sc to the alloy enhance ductility, the hardness, yield
strength and upper tensile strength up to 30%, 20%, 20% and 25% respectively. When the
studies carried out within the scope of the thesis are compared with the literature review, it has
been observed that the addition of Sc does not cause a noticeable change in the hardness value
of the alloy. According to the results obtained in the study, the most ideal addition rate is 0.25
wt.% Sc, and it has been obtained that an increase in this rate leads to a deterioration in the
mechanical properties of the alloy. The results found in this study are consistent with the
literature.

36
4.5 Hardness
The variation of Vickers hardness of gravity cast Al-6.8Sc alloy, gravity cast Al-Mg-Sc alloy
and Squeeze cast Al–Mg–Sc alloys of different composition and conditions were found using
Wilson hardness tester (Wilson VH1202). Although the average hardness of Al-Mg-Sc alloy
obtained is 82.33Hv, the average hardness value of gravity cast Al-Mg-Sc alloy is found to be
55.33Hv at a load 300g and that of gravity cast Al-6.8Sc is given as 63.66Hv at 300g load.
Apparently, it can be said that the presence of Sc in a greater content in alloy Al-6.8Sc could
have helped to produce a larger hardness than that of gravity Cast Al-Mg-Sc which has a lesser
content of Sc, but the same Al-Mg-Sc alloy prepared through squeeze casting process gives
even greater hardness value. In particular, the increase in hardness value by approximately 20%
can be noted by Al-Mg-Sc alloy prepared through squeeze casting process.
90

75
Hardness (HV0.5)

60

45

30

15

0
Al-6.8% Al-Mg-Sc Al-Mg-Sc
Sc Gravity Sqeeze
Die Cast Cast
Alloy

Mean Hardness Error

Figure 4.12: Vickers hardness measured for Squeeze cast Al-Mg-Sc alloy, gravity cast Al-Mg-
Sc alloy and gravity cast Al-6.8Sc alloys.

37
 CONCLUSION
• Microstructures characterizing the binary Al-2021, Al-6.8Sc, Al-5Mg-0.25Sc prepared
by conventional gravity cast method and Squeeze cast Al-Mg-Sc were formed by the
Al matrix and eutectic mixture of α-Al + Al3Sc possessed a complete hypoeutectic
structure demonstrated by globules containing eutectic α-Al in the form of dendrites.
Al-Mg-Sc sample produced through gravity casting process, as well as the Squeeze cast
method displayed a mixture of hypoeutectic and eutectic characteristics with α-Al
matrix cells within the structure, whereas for Al-6.8%Sc prevalence of a complete
eutectic structure was seen to occur. Thus, the eutectic composition of Al-Sc binary
stand between 1 and 7 wt.% Sc.
• The Squeeze cast Al-Mg-Sc alloy has shown to have a comparatively greater micro
hardness about 20% in hardness to that of Al-6.8Sc alloy. This hardness value
improvement has been attributed to the increasing volume fraction of α-Al matrix and
the Al3Sc matrix combined precipitates present. The micro hardness of the Al-Sc binary
system is found to be influenced by the addition Mg, and production process changed
to squeeze cast has greatly influenced the hardness of the system.
• In comparison of experimentally obtained micro hardness data with that of the literature
of other Al Alloy system such as Al-Co, Al-Cu-Mn, Al-Zn-Mg-Cu systems has shown
a longer and better stability.

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