ABSTRACT

Metal Matrix Composites (MMC) find their presence well in the place
where monolithic metals and alloys fall short to meet the requirements.. MMCs
were widely used in the application areas where enhanced properties are required
such as high stiffness-to-weight ratio in aerospace industries, high corrosion
resistance in marine applications, good temperature workability in space
applications etc., Friction Stir Welding (FSW) process is an emerging solid state
joining process in which the material that is being welded, does not melt and recast.
Friction stir welding creates the weld joint without bulk melting. In addition, the
extensive thermo mechanical deformation induces dynamic recrystallization and
recovery that refine the microstructure in the stir region.

Al 6063 Aluminium alloy was added with the reinforcements, Silicon

Carbide and Boron Carbide for the manufacturing of the proposed Aluminium
Matrix composite through liquid processing technique (Stir casting). The HMMCs
containing different weight % (5, 10 and 15) of Si C and 10% of B 4C was
manufactured. The microstructure and mechanical properties of the fabricated metal
matrix composites were analysed. The good dispersion of B4C and SiC particles in
the matrix was observed from the micrographs taken with optical microscope and
scanning electron microscope. The mechanical properties like hardness and tensile
strength were improved with the increase in weight percentage of Si C and B 4C
particulates in the Aluminium matrix hybrid composite. The best results were
observed for the fabricated aluminium matrix hybrid composite reinforced with Si
C and B4C (each 10%). In this investigation, a tool rotation speed of 1000 rpm for
Al 6063 hybrid metal matrix composites are found to be optimum to get maximum
tensile strength of friction stir welding joints. The friction stir welding joint
fabricated at a lower tool rotational speed of 800 rpm have exhibited lower tensile
strength. The joint fabricated at a tool rotational speed of 1000 rpm yielded higher
tensile strength. Similar observations were observed for hardness also.
 ii

LIST OF SYMBOLS AND ABBREVIATIONS

Al - Aluminium

AMC - Aluminium Matrix Composites

Al2O3 - Aluminium Oxide

ASTM - American Society for Testing of Materials

ANOVA - Analysis of Variance

AL - Axial Force

BM - Base Metal

BM - Base Metal

B4C - Boron Carbide

BN - Boron Nitride

CMC - Ceramic Matrix Composites

CFAMC - Continuous fiber-reinforced AMC

FSW - Friction Stir Welding

HAZ - Heat Affected Zone

MPa - Mega Pascal

MMC - Metal Matrix Composites

μm - Micrometer

μm - Micrometre

ml - Millilitre

mm - Millimetre

OM - Optical Microscope

PAMC - Particle-reinforced AMC

PMC - Polymer matrix composites

 iii

RSM - Response surface methodology

RSM - Response Surface Methodology

RS - Retreating Side

Hv - Vickers Hardness

SEM - Scanning Electron Microscope

SEM - Scanning Electron Microscope

SFAMC - Short or Whisker fiber-reinforced AMC

SiC - Silicon Carbide

SZ - Stir Zone

TMAZ - Thermo Mechanically Affected Zone

Ti - Titanium

TiB2 - Titanium Boride

TRS - Tool Rotation Speed

UTS - Ultimate Tensile Strength

Wt % - Weight Percentage

WS - Welding speed
 1

CHAPTER 1

1 INTRODUCTION

1.1 COMPOSITE MATERIALS

Materials have had a huge impact on the evolution of the human race.
The cultural record of man’s existence is divided into two great periods – the ‘Age of
Stone’ and the ‘Age of Metal’. The Stone Age was a broad prehistoric period during
which stone was widely used to make implements with an edge, a point, or a
percussion surface. The period lasted roughly 3.4 million years and ended between
8700 BCE and 2000 BCE with the advent of metalworking. Metal was first used in
Asia and Egypt about 3500 BC, and in Europe about 2000 BC. Once the use of metal
was recognized, the city-life and also an infinite variety of inventions took place
which contributed to the rise of human civilization. Metal enhanced man’s mastery
with stone, wood and other substances.

In ancient days bricks made of clay reinforced with straw were used as
composites. Conventional monolithic materials have restrictions to meet today’s
demands in the field of advanced technologies. Evolution in the field of material
science has led to the birth of composite materials. Today composite is becoming an
essential part due to its high strength-to-weight ratio and high stiffness-to-weight
ratio. Many composites employed nowadays are at the leading edge of materials
technology with their performance and costs suitable for applications such as
spacecraft, automobile, etc.,. These materials combine the best features of various
materials to improve its physical and mechanical properties.
 2
Classification of composites

Composites can be broadly classified according to the matrix materials

(as polymer matrix composites, metal matrix composites and ceramic matrix
composites) and morphology of reinforcements (particulate, fibre, whisker, laminate
and woven). Suitable selection of matrix materials, reinforcement and composition
leads to the wide range of microstructures in composites which also includes the
isotropic and anisotropic behaviour.

Hybrid metal matrix composites

When at least two reinforcements are present in the metal matrix the
composite is known as Hybrid Metal Matrix Composite (HMMC). They are prepared
by dispersing two or more reinforcing materials into a metal matrix and received
considerable research and trials by Toyota Motor Inc., in the early 1980s. The lighter
metals such as aluminium, titanium are used as matrix and the reinforcement
materials are embedded into the matrix to enhance the physical properties.

Aluminium metal matrix composite reinforced with SiC and B4C

particulates are new range of advanced materials. The presence of reinforcements
(SiC, B4C and Al2O3 etc.,) in HMMCs results in the improvement of wear resistance
and strength to weight ratio than the unreinforced alloys HMMCs can effectively
compete with super alloys, ceramics and plastics toward the development of high
performance composites with high strength. HMMCs are suitable for applications,
which oblige characteristics such as combined strength, damping properties, thermal
conductivity and co-efficient of thermal expansion with lower density. It is found that
the applications of HMMCs in aerospace industries and automobile parts such as
drive shafts, cylinders, pistons and brake rotors, consequently create interest in
studying wear behaviour of the structural components
 3
Types of reinforcements in composites

Reinforcement enhances the stiffness, strength, resistance to temperature

and reduces the density of composites. To achieve these properties, the selection of
reinforcement material should be based on the type of reinforcement, production
methodologies and chemical compatibility with the base matrix alloy. The various
types of reinforcements employed in composites are shown in Figure 1.1

Figure 1.1 Classifications of reinforcements

 4
1.2 APPLICATIONS OF COMPOSITE MATERIALS

The composite materials are used in a wide range of application due to

their effective thermal, mechanical, and electrical properties and also their matching
adaptability to the requirements.

 Automobile body panels.

 Structural applications.

 Aerospace applications.

 Light weight industrial materials.

 Marine structures.

 Bio-medical equipment.

 Mechanical parts & machinery.

 Electrical & Electronic communication applications.

 Power, Energy generation & Transmission equipment.

1.2.1 Characteristics of metal matrix composites

Metal matrix composites comprise of a metallic alloy reinforced with

ceramic particulates or fibres. The addition of reinforcements in the matrix alloy
caters the composites with properties not attainable with monolithic alloys. The main
functions of a base alloy are to transfer the load to the reinforcement, hold the
reinforcement and to protect the composites from mechanical or chemical damage.
The important functions of reinforcement is to carry the applied load and to delay the
dislocation motion in dispersion form. Metal matrix composites are more
advantageous than conventional monolithic metals in the following aspects
 5
 Increased specific strength

 Improved wear resistance

 Improved damping capabilities

 Good corrosion resistance

 Higher strength to weight ratio

 Better fatigue resistance

 Better elevated temperature Properties

 Lower coefficient of thermal expansion

Some of the commonly employed materials in metal matrix composites are

Matrix - Aluminium, Magnesium, Copper based alloys, Iron etc

Reinforcement – Silicon Carbide, Boron Carbide, Zirconium, Aluminium Oxide,

Tungsten carbide, etc.,.

Aluminum matrix composites

Aluminium is widely used as a base alloy for metal matrix composites.

These alloys are quite fascinated because of its properties such as low density, good
corrosion resistance, high electrical and thermal conductivity and better fatigue
resistance. Aluminium Matrix Composites (AMCs) have been extensively used in
automotive, aerospace, defence, sporting goods, electronic packaging industries. The
properties can be tailored by varying the constituents and its volume fractions. The
commonly used reinforcements are SiC, Al2O3, B4C, SiN, etc.,. AMC’s provide
excellent combination of properties in such a way that the monolithic material cannot
be a competitor. Over the decades, AMCs have been experimented and used in a
number of structural, non-structural applications in various engineering fields. The
usage of AMC in these sectors is mainly due to its performance, financial and
environmental benefits. The major benefits of AMCs are in the automotive sector
due to the lower fuel consumption, less weight and lower emissions. Lack of material
 6
knowledge, information about the different manufacturing methods and possibility of
utilisation has hindered the usage of AMCs.

Boron carbide (b4c) as reinforcement

Boron carbide (B4C) is one of the hardest ceramic materials that can be
used in the manufacture of ballistic armour, vehicle armour and multi industrial
applications. Boron carbide particulates are generally produced by reacting carbon
with B2O3 in an electric arc furnace by carbo thermal reduction.  The harder nature,
low density of boron carbide helps in increasly the strength and hardness of the
composites.

Silicon carbide (sic) as reinforcement

Silicon carbide (SiC) particulates have been used as reinforcement

material as it is the only chemical compound of carbon and silicon. It has been
originally produced by a high temperature electro-chemical reaction of carbon and
sand. Silicon carbide has been an excellent abrasive and thus made into grinding
wheels and other abrasive products for over hundred years. This material has now
been developed into a high quality technical grade ceramic with very good
mechanical properties. It has been used in refractories, abrasives, ceramics and
numerous high-performance applications.

Production and processing of HMMCS

Hybrid Metal Matrix Composites (HMMCs) can be developed by many

diverse techniques. Based on the type of reinforcement, size and morphology, the
HMMCs have been fabricated by different methods such as stir casting, squeeze
casting, spray deposition, liquid infiltration, powder metallurgy, etc.,
 7
STIR Casting

Stir casting set-up is one of the liquid phase fabrication method mainly
consists of a furnace and a stirring assembly as shown in Figure 1.2. In general, the
solidification synthesis of HMMCs involves a melt of the selected matrix material
followed by the introduction of a reinforcement material into the melt, obtaining a
suitable dispersion. The next step is the solidification of the melt containing
suspended dispersions under selected conditions to obtain the desired distribution of
the dispersed phase in the cast matrix.

Figure 1.2 Schematic diagram of stir cast method (Huda et.al.1993)

In preparing hybrid metal matrix composites by stir casting method, there

are several factors that need considerable attention, including,

 Difficulty in achieving a uniform distribution of the

reinforcement material.

 Wettability between the two main substances.

 Porosity in the cast metal matrix composites.

 Chemical reactions between the reinforcement material and the

matrix alloy.
 8
In order to achieve the optimum properties of the HMMCs, the
distribution of the reinforcement material in the matrix alloy must be uniform and the
wettability or bonding between these substances should be optimized. The porosity
levels need to be minimized.
 9

CHAPTER 2

LITERATURE REVIEW

This chapter provides a review of past research efforts related to

composites, reinforcement particles, mechanical properties, and friction stir welding
process parameters of metal matrix composites (MMCs). Composite structures have
shown universally a saving of at least 20% over metal counterparts and a reduced
operational and maintenance cost

Literature survey reveals that most of the engineering applications

demand high strength, light weight and high resistance to corrosion. The main reason
behind the popularity and development of Hybrid Aluminium Metal Matrix
Composites (HAMMCs) is that aluminium and its alloys have good strength to
weight ratio and good corrosion resistance.

In the present scenario, researchers have mainly been focused on

aluminium metals for automotive applications because of its unique combination of
corrosion resistance, low density and excellent mechanical properties as compared to
other metals. In addition, literature also reveals that most of the published works
have considered aluminium based composites due to their low density, wide alloy
range, heat treatment capability and processing flexibility.

The properties of the matrix play a vital role in the selection process.
Generally, Al, Ti, Mg, Ni, Cu, Pb, Fe, Ag, Zn, Sn and Si are preferred as the matrix
material, among which Al, Mg and Ti have been used widely. Along with the basic
properties required for a material to behave as a matrix, magnesium-based systems
also possess lower elastic modulus. Magnesium often results in a higher
improvement in the properties with reinforcements than that of aluminium, although
many of the composite fabrication processes have been common to both Al and Mg-
based systems . Magnesium and magnesium alloys are among the lightest materials
for practical use as a matrix phase in MMCs. However, it has been reported by
 10
several that though their low density makes them competitive in terms of
strength/density values, magnesium alloys are not good competitors for aluminium
alloys in terms of absolute strength.

The reason for aluminium being a successful matrix material over

magnesium is said to be mainly due to the design flexibility, good wettability and
strong binding at the interface. Among the enormous varieties of aluminium alloys,
Al 6063 was preferred as a better choice, because of the formability characteristics
and the possibilities of modifying the strength of the composite by employing
optimal heat treatment.

(T. Senthilnathan and K. Balachandar 2018) successfully used stir

casting technique was to fabricate AA7475/B4C/CeO2 composites and observed that
no clusters of reinforcement particles. Moreover improved mechanical properties of
the AA7475 metal matrix composite was observed upon addition of B 4C particles as
reinforcement and had adverse effect with CeO2 and hybrid composite with (B4C +
CeO2) particles as reinforcement resulted in optimum tensile strength and ductility.

(Li et al 2018) observed that FSW resulted in obvious homogenization and

fragmentation of B4C, thereby remarkably increased the hardness of the nugget zone.
The hardness profiles of the welded joints were hardly influenced by B4C contents
but significantly by the welding speeds. “S” line and a B 4C depleted region were
formed at the top and the bottom of the nugget zone (NZ), respectively. However,
they did not deteriorate the mechanical properties of the joints. The tensile strength
of all the joints was close or even up to that of the base material with the fracture
occurring at the base material.

(Saurabh Kumar Gupta.et.al 2018), studied friction stir welding (FSW) is a

solid state joining process and one of the most promising technique for defect free
joining of aluminium alloys. Genetic algorithm-based optimisation of FSW process
parameters is used for joining of dissimilar AA5083-O and AA6063-T6 aluminium
alloys. For genetic algorithm based process parameter optimisation, regression
models were considered as objective functions. The regression models have been
 11
found satisfactory for predicting the responses at 99% confidence level. The derived
set of optimal process parameters were found as tool rotational speed of 900 rpm,
welding speed of 60 mm/min, shoulder diameter of 18 mm

(Ravi Kumar et.al. 2018) studied to fabricate Al 6063 based hybrid

composites with reinforcements SiC and B4C using the conventional stir casting
method. The hybrid composites further processed with the FSW process and the
performance was analysed to find out metallography and mechanical properties. The
hybrid composites were compared with unreinforced alloy in terms of physical
properties and check the suitability for structural components in automotive
applications

(Kaviyarasan, K et.al. 2018) identified the physical and mechanical

performance of Al2O3 and B4C reinforcement with Aluminium 7075 matrix prepared
by using a modified stir casting method. The HMMC comprises the base matrix
Aluminium 7075 with different concentrations of two particles reinforcements Al 2O3
and B4C. In the first study, B 4C was kept with a constant weight percentage and wt%
of Al2O3 was varied along 2,4,6,8 and 10. In the second study, wt% of Al 2O3 was
constant and that of B4C was kept at 5 wt% for the sample specimens.

(Pridhar et.al. 2018) determined the metallurgical and mechanical properties

were analyzed from ZrO2 and the coconut shell ash particles in Aluminium 6082
MMCs. The weight percentage of coconut shell ash particles, ZrO2 were varied from
the value of 0 to 10 wt% and fabricated by stir casting techniques .

(Salih, et. al.2019) demonstrated that the overall quality FSW joints is highly
influenced by welding parameters (tool rotation and welding speeds). The use of
higher weld pitch leads to an increase in the tendency of formation of tunnel defects,
cavity and incomplete penetration in the FSW joints, as a result of insufficient plastic
flow, mixing time and heat input.

(Ramachandrana and Murugan 2019) in their work, 3 mm thick Al alloy

AA5052-H32 and HSLA steel IRS-M42-97 were successfully butt welded using
FSW technique. They have taken trials by varying the axial force from 4 to 9 KN
 12
while keeping the other FSW parameters constant. They observed that the highest
joint strength of 189 MPa (about 90% of the UTS of the base Al alloy) is obtained at
7 KN axial force. The range of axial force that could produce joints with good joint
strength (above 75% of UTS of the base Al alloy) is very narrow.

(Jayaseelan et. al.2019) made a detailed investigation in friction stir welding

aluminium metal matrix compositesusing tools of different profiles. viz. plain
pentagon, plain tapered and threaded cylinder, materials viz. OHNS, HCH Cr, H13
and D/d ratio 2, 3 and 4, on a commercial CNC enabled FSW machine. From this
result it was recommended that the effect of tool profile makes a major role to decide
the weld joint towards producing quality welds using FSW process.

(K.S. Sreenivasan et..al. 2019), studied that the friction welding of

aluminium metal matrix composite AA7075-10 vol% SiCP-T6 Genetic Algorithm
approach had been applied to optimize the friction welding process parameters
depending on the weights given to the Ultimate Tensile Strength and Hardness. The
Genetic Algorithm predicted optimized process parameters were validated by
conducting the friction welding on the Aluminium metal matrix composite
subsequently the Ultimate Tensile Strength and Hardness were experimentally found,
and it showed the values with acceptable deviation.

(Dwivedi et al.2019), observed that the tensile strength and hardness were
improved by adding the Si C and Al2O3 ceramic particles in aluminium 6061.
However, toughness was reduced by adding the Si C and Al 2O3 ceramic particles in
aluminium alloy. They also observed that hard ceramic particles Si C and Al 2O3
ceramic particles enhanced hardness significantly, but toughness reduced.

(Pugalenthi et al. 2019), in his research work found that stir casting is an
effective technique to produce hybrid metal-matrix composites with good miscibility.
He also observed that the tensile strength and yield strength of the Si C & Al 2O3
filled Al 7075 alloy composites were found to increase with an increase in the
reinforcements
 13
A number of practical applications have been produced by the liquid state
processes because of their inherent advantages, which includes low cost, better
handling ability of the liquid metal compared to powders and ability to produce these
composite parts by the conventional casting methods. There are four major processing
techniques in liquid state processes.

 Stir-Cast
 Infiltration Process
 Spray Deposition
 In-situ Fabrication

Influence of tool rotational speed on FSW process.

Effect of tool rotational speed on microstructure

The precipitates redistribution and recrystallized grain structure in the

weld nugget zone indicated that lower than the melting temperature but the
temperature was higher than the solution temperature The wider weld zone near the
upper surface due to the excess deformation and frictional heating generated during
the welding. The region between 12.5 and 10 mm from the weld centre has a less
concentration of needle-shaped precipitates. All precipitates within 8.5 mm from the
weld center region get dissolved. The low concentration of needle-shaped
precipitates leads to the softening of the weld.

Effect of Tool Rotational Speed on Tensile Strength

(Zhang et. al.2019) studied friction stir welding to assess the influence
of rotational speed (600, 950, 1300 and 1650 rpm) on the microstructure features,
materials flow and mechanical properties. The results indicated that low rotational
speed leads to a limited materials mixing, while the typical onion ring of mixing
pattern can be acquired at the high rotational speed. Compared to the base materials,
 14
significant grain refinement occurs in all the joints at a rotational speed of 600 rpm.
Increasing the rotational speed is prone to result in grain coarsening.

(Acharya et. al.2019) investigated the effect of tool rotational speed (TRS)
on the mechanical property of friction stir welded joints of AA6092/17.5 SiCp-T6
composite. 6 mm thick plates are welded at a constant tool traverse speed of 1 mm/s
by varying the TRS at 1000 rpm, 1500 rpm and 2000 rpm. The migration of particles
has been encountered at higher TRS (2000 rpm). The microhardness analysis depicts
variation in average hardness from top to bottom of the NZ, minimum for 1500 rpm
and maximum for 2000 rpm. The impact strength at 1000 rpm and 1500 rpm remains
close to that of BM (21.6 J) while 2000 rpm shows the accountable reduction. The
maximum joint efficiency has been achieved at 1500 rpm (84%) and minimum at
1000 rpm (68%) under tensile loading.

Effect of Tool Rotational Speed on Hardness

(Rajakumar et al. 2018) observed that irrespective of the tool rotational

speed the hardness value in the Stir Zone was higher than that of the base metal
because of fine grain size and small particles of intermetallic compounds. The higher
hardness value of 203HVwas recorded in the Stir Zone for the joint fabricated with a
tool rotational speed of 1400 rpm

The following research problem has been identified from the review of
available literature.

In aluminium based MMCs, a lot of effort has been done with different
types of reinforcements varying the size and manufacturing techniques

When the percentage of reinforcement increases in the matrix, the

hardness and wear resistance of composite increases.

Now, the significant part of efforts in aluminium matrix composite has

been directed towards the development of high-performance composites with high
strength and good mechanical properties for using in the automotive and aerospace
 15
applications. The Al 6063 matrix composite reinforced with SiC and B4C
particulates has been a new range of advanced material because of the potential
improvement in mechanical properties such as hardness and tensile strength. This
greatest improvement in the mechanical properties has generally been obtained by
means of reinforcement with appropriate particulates. Most of the research work has
been reported on Al 6063 with different reinforcement such as silicon carbide,
silicon, boron carbide, titanium, alumina, etc. But none of them had attempted for Al
6063 with two types of reinforcements like SiC and B4C.

CHAPTER 3

FABRICATION AND CHARACTERIZATION OF Al 6063-

SiC - B4C- HMMC

INTRODUCTION
Hybrid metal matrix composites (HMMCs) are competent materials to be
employed in various applications in industry because of their properties. A range of
HMMC materials has been studied to combine the desirable attributes of ceramics
and metals. The suitable fabrication procedure with excellent mechanical properties
of these materials and their relatively lower production cost make them attractive for
a variety of applications in aerospace and automotive industries.

This chapter describes the fabrication process and the characterization of

Al 6063 based HMMC reinforced with SiC and B4C as a particulate material. The
microstructures and mechanical properties such as tensile strength and hardness of
the HMMCs produced are detailed in this chapter

6063 Aluminum alloy

Aluminum alloys with a wide-ranging of properties are used in

engineering industries. Alloys are classified by a number system (ANSI) or by names
indicating their main alloying constituents (DIN and ISO). Selecting the right alloy
for a given application entails considerations of its density, ductility,
 16
formability, tensile strength, yield strength, workability, weldability and its corrosion
resistance. Aluminum alloys are used in different fields due to their high strength-to-
weight ratio. Pure aluminum metal is only used in non-structural applications, as it
does not have the high tensile strength that is needed. Applications with industrial
requirements most frequently use aluminum 6063 alloy (Al – 97.65 %, Si – 0.6 %, Fe
– 0.35, Cu – 0.1, Mn – 0.1 % and Mg – 0.9 %. Zn – 0.1, Ti – 0.1, Cr – 0.1). It is used
in ship manufacturing due to its high strength and bearing capacity to sea
atmosphere. It is also used in nuclear industries. It finds extensive use in numerous
specific applications such as engine cylinders, pistons, manifolds and motor casings.

Silicon Carbide

The Mohs hardness of Silicon Carbide is 7 and its melting point is around
27300C. It is composed of tetrahedral lattice structure and carbon and silicon atoms
have strong bonds in the crystal lattice. This produces a hard and strong material. It is
not attacked by any acid or alkali or molten salt up to 800°C.

In air, Silicon Carbide forms a protective silicon oxide coating at 1200°C

and is can be used up to 1600°C. The thermal conductivity coupled with low thermal
expansion and high strength gives an exceptional thermal shock resistant qualities to
the material. SiC ceramics with no grain boundary impurities maintain their strength
at very high temperatures with no strength loss.

Silicon Carbide is an excellent abrasive and has been used in grinding

wheels and in other abrasive products for over one hundred years. Today, the
material has been developed with a high quality technical grade ceramic with good
mechanical properties. Silicon Carbide has low density, high hardness and high
strength and hence, it is used in wide range of high-performance applications.

Boron Carbide

B4C is a crystalline compound of boron and carbon. It is an extremely

hard and synthetically fabricated material that is also used in abrasive and wear-
 17
resistant products, in lightweight composite materials, and in control rods for nuclear
power generation.

The Mohs hardness of B4C is 9.5 and its melting point is around 2450 0
C.It is one of the hardest synthetic substances and is being exceeded only by cubic
boron nitride and diamond. In abrasive, it is used in powdered form in the lapping of
metal and ceramic products, though its low oxidation temperature makes it unable to
withstand the heat of grinding hardened tool steels. Due to the hardness and very low
density, it has been used as a reinforcing agent for aluminum metal matrix
composites in high- performance bicycles and military armor, and its wear resistance
has caused it to be employed in sandblasting nozzles, pump seals etc.,. Being a
neutron absorber, boron carbide is used in powdered form to control the rate of
fission in nuclear reactors.

Fabrication Process of Al6063 –SiC -B4C HMMC

The proposed Al - SiC - B4C HMMC was produced by stir casting

process. Al 6063 alloy was used as a matrix B4C with a size of 30 microns and
silicon carbide with a size of 33 microns were used as a reinforcements, K2TiF6
(Potassium fluotitanate) was used for enhancing the wettability of SiC and B4C with
Al melt during stir casting process. The chemical composition and the properties of
Al 6063 is given in Tables 3.1 and 3.2 respectively.

Table 3.1 Chemical Composition of Aluminum Alloy (6063)

Elements Mg Si Fe Cu Mn Cr Zn Ti Al

% by
0.9 0.6 0.35 0.1 0.1 0.1 0.1 0.1 Balance
Weight

Table 3.2 Properties of Matrix and Reinforcement Materials

Al B4C SiC
Property

Density (g/cm3) 2.69 2.52 3.21

 18

Melting point (ºC) 615 2763 2730

Coefficient of thermal expansion(10-6/ºC) 23.4 5.0 4.0

Young’s modulus (GPa) 68.3 450 410

Aluminium alloy was melted in stainless steel crucible at 750°C using an

electrical resistance furnace. Figure 3.1 shows a typical stir casting set up. The melt
was agitated with the help of a mechanical stirrer to form a vortex (Hashim et al
1999, Sevik et al 2006). The mixtures of preheated SiC and B4C particles with
K2TiF6 flux were added at a constant feed rate into the vortex. Stir casting equipment
having the provision for transferring the melt into a mold was used. After the stirring
process the molten mixture, was poured down into the preheated permanent mold.
The HMMCs having different weight percentages (5, 10 and 15) of SiC and 10
percentage weight of B4C were fabricated by the same procedure. The maximum
amount of B4C was limited up to 10% due to the formation of higher amount of slag
on the melt surface which caused the inclusions in the trial castings. The
manufactured HMMCs are shown in Figures 3.2.

Mechanical Stirrer Assembly

The material of the stirrer rod and impeller is made of stainless steel
because of its high corrosion resistance and creep properties. The stirrer was driven
by a variable speed motor (range of speed 50-1800 rpm) to mix the reinforced
particles with the aluminium alloy. An inbuilt lifting system was used to lower or
raise the stirrer in melt surface which facilitated the stirrer positioning, replacement
and cleaning purpose. The impeller blades were designed in such a way that it create
a good vortex to complete thorough particle mixing. Impeller consisting of four
blades at 90° angle to each other was selected for this research work. The impeller
blades were coated with graphite material to minimize blade dissolution in molten
metal. The stirring speed should not be too high, but should be constant for a few
minutes before the molten metal was poured into a die. The stirrer assembly was also
preheated to remove other contaminations and moisture before each start-up.
 19

Figure 3.3 Stir casting set up

Figure 3.4 Fabrication of Al 6063-B4C -S i C Composites by stir casting

Evaluation of metallurgical and mechanical properties of HMMCS

Evaluation of Microstructure

Metallurgical characterization of fabricated hybrid metal matrix

composites was carried out using an optical microscope, scanning electron
microscope. The specimen prepared from the hybrid metal matrix composites were
 20
polished and etched as per the standard metallographic procedure. The etchant used
to reveal the microstructure in this study consisted of 3 g sodium molybdate, 5 ml
HCl (35%) and 2g ammonium bifluoride in 100 ml distilled water. The specimen
were immersed in the etchant at room temperature until the surface was etched and
dried in hot air later.

Optical Microscopy

The microstructures of the etched specimen were observed using a

metallurgical microscope. Photomicrographs were taken on the top surface of hybrid
metal matrix composites specimen.

Scanning Electron Microscopy

The microstructures of etched hybrid metal matrix specimen were

observed using a SEM.

Evaluation Of Mechanical Properties

Hardness test

To evaluate the hardness of the hybrid metal matrix composites

composites, the hardness test was conducted. The microhardness of polished samples
was measured at different locations using the Vickers hardness tester

Tensile test

The tensile tests were used to assess the mechanical behaviors of the
HMMCs. The tensile specimen were prepared from the cast composite as per ASTM
E08 standard. The dimensions of the specimen is shown in Figure 3.3. The ultimate
tensile strength was estimated using a computerized universal testing machine. Three
specimen prepared from each HMMCs and base alloy as shown in Figure 3.4 were
tested and the average value of tensile strength was determined.
 21

Figure 3.5 The dimensions of tensile specimen.

Figure 3.6 Tensile Specimen of Al 6063–B4C –S i C Composites (a) Before

Fracture and (b) After Fracture

Aluminum reinforced with SiC and B4C particulate composites are

successfully fabricated by a stir casting process. The addition of K2TiF6 flux has
improved the wettability of SiC and B4C particles with molten aluminum and
facilitated the incorporation of SiC and B4C particles in the Al matrix. The flux reacts
with the melted surface of SiC and B4C particle and produces Ti layers around the
surface of SiC and B4C particles. This reaction is exothermic in nature and heat is
evolved in the vicinity of SiC and B 4C particle-melt interface which enhances the
incorporation of particles into the melt (Kennedy and Brampton 2001).
 22

Evaluation of Microstructure

Optical Micrograph

The optical photomicrographs of the cast Al 6063 alloy and the fabricated hybrid
metal matrix composites are shown in Figures 3.5. It shows the microstructure of
cast Al 6063 alloy exhibiting a typical dendritic structure. In most wrought
aluminium alloys, solidification begins with the development of a dendritic network
of primary aluminum. The secondary dendritic arm spacing is essentially
determined by alloy composition, local solidification time, cooling rate and
temperature gradient.

The mechanical properties of the wrought alloys are determined

primarily by the secondary dendritic arm spacing and the morphology of
interdendritic phases in their microstructure.

Figure 3.7 A Photomicrograph of Al 6063 Alloy

 23
Scanning Electron Microscopy

Figures 3.6 shows scanning electron micrograph of fabricated Hybrid metal

matrix composites. The SEM images reveal that the homogeneous dispersion of SiC and
B4C particles in the matrix. During the solidification of composites the aluminum
dendrites solidify first and the SiC and B4C particles are rejected by the solid-liquid
interface. Hence, the particles are segregated at the inter dendrite region. Ti reaction
layer was formed when adding K2TiF6 flux into the melt where K and F contributed
for removing the oxide film from the Al surface . The weak reaction layer in the
region was not so clear in the SEM image due to the removal of interface.

SiC

B4C

Figure 3.8 SEM Photomicrograph of Al 6063-10 % wt. B4C and 10% wt of

SiC HMMC

Evaluation of Mechanical Properties

The estimated mechanical properties of HMMCs are presented in Table 3.4.

 24
Table 3.3 Mechanical properties of manufactured Al 6063 –SiC and B4C
composites

Sl.No % of SiC % of B4C Ultimate Yield Hardness Elongation

in Al tensile Strength
in Al matrix strength (Hv) %
matrix (MPa) (N/mm )
2

1 5 10 205.6 190.5 82 3.03

2 10 10 225.1 205..6 93 2.86

3 15 10 223.5 200.2 95 3.17

Hardness Test

The mechanical properties of matrix alloy Al 6063 is improved upon SiC

and B4C incorporation. Figure 3.7 shows the effect of weight percentage of SiC and
B4C reinforcement particulates on the hardness of fabricated hybrid metal matrix
composites. It is observed that the microhardness of metal matrix composites linearly
increase when the amount of reinforcement particulates increases. Addition of
reinforcement particles in the matrix increases the surface area of the reinforcement.
The presence of such hard surface area of particles offers more resistance to plastic
deformation which leads to increase in the hardness of composites. It is reported
(Ramesh et al. 2009) that the presence of hard ceramic phase in the soft ductile
matrix reduces the ductility of composites due to reduction of ductile metal content
which significantly increases the hardness value.
 25

Al 6063 HMMC
98
Hardness Number(Hv)
95
92
89
86
83
80
0 5 10 15
SiC(Wt.%)+B4C 10 wt% Content

Figure 3.9 Effect of B4C and Si C Particulates on the Hardness of Al 6063-

B4C and SiC metal matrix composites.

Tensile Test

Figure 3.8 shows the effect of the weight percentage of SiC and B4C
particulates on tensile strength. It can be inferred that SiC and B4C particles are very
effective in improving the tensile strength of composites. It is due to the
strengthening mechanism of the reinforcement (Feng et al. 2009). The addition of
SiC and B4C particles in the matrix induces much strength to matrix alloy by offering
more resistance to tensile stresses. It is well known that the thermal expansion
coefficient of SiC particle is 4x10-6/ºC and B4C particle is 5x10-6/ºC and for
aluminum alloy is 23x10-6/ºC.

The thermal mismatch between the matrix and the reinforcement causes
higher dislocation density in the matrix and load bearing capacity of the hard
particles which subsequently increase the composite strength (Toptan et al. 2010).
 26

Al 6063 HMMC
230
Ultimate Tensile Strength (Mpa)
225

220

215

210

205

200
0 5 10 15 20
SiC(Wt.%)+B4C 10 wt% Content

Figure 3.10 Effect of B4C and SiC Particulates on UTS of Al 6063-B4Cand SiC
metal matrix composites

Fabrication of Hybrid Metal Matrix Composites with SiC and B4C

particles by casting process is usually difficult because of the poor wetting between
Al 6063 with SiC and B4C agglomeration phenomena which result in weak
mechanical properties. In the present work, Al 6063 aluminum alloy matrix
composites reinforced with B4Cand SiC particles were produced by stir casting route.

Titanium containing flux (K2TiF6) was used to increase the wetting

between Al 6063 hybrid metal matrix composites,which facilitate the incorporation
of SiC and B4C particles into molten aluminum. The HMMCs containing different
weight % (5, 10 and 15) of SiC and 10% of B 4C was manufactured. The
microstructure and mechanical properties of the fabricated metal matrix composites
were analyzed. The good dispersion of B 4C and SiC particles in the matrix was
observed from the micrographs taken with optical microscope and scanning electron
microscope. The mechanical properties like hardness and tensile strength were
improved with the increase in weight percentage of SiC and B4C particulates in the
Aluminum matrix hybrid composite.

Friction stir welding is a solid-state welding process, generates

coalescence at temperatures lesser than the melting point of the base materials being
 27
joined. In friction stir welding rotating tool moves all along the joint interface, heat is
generated which results in a re-circulating flow of plasticized material close to the
tool surface. Due to the rotational and transverse movement of the friction stir
welding tool, the softened material was extruded, the stir zone was formed. The
material flow performance under the action of the rotating tool affects the formation
of the stir zone. In friction stir welding various researchers has taken a huge effort to
know the influence of predominant process parameters on the material flow
behaviour and mechanical properties of the welded joint. Selecting the most effective
friction stir parameters and comprehending the influence of the process parameters
on the weld properties has been major active topics for many researchers This
chapter presents the experimental procedure followed for friction stir welding of Al
6063 metal matrix composite, selection of friction stir welding process parameters
and fabrication of friction stir welding tool. The procedure and the equipment used
for evaluating the friction stir welding joints are also described. The effect of various
friction stir welding process parameters such as tool rotational speed, welding speed
or feed and the axial force on the metallurgical and mechanical properties are also
presented.

Identifying fsw process parameters and fabrication of FSW tool

Tool rotational speed, welding speed, and the axial force were the most
prominent friction stir welding process parameters which influence the mechanical
and metallurgical properties of friction stir welds In addition to the above mentioned
parameters, the profile of the friction stir welding tool pin also plays an important
role on the mechanical properties of the friction stir welded joints which decides the
material flow between the workpieces during friction stir welding.

The friction stir welding tool was manufactured with the help of CNC
lathe and wire cut EDM machine. Cylindrical shoulder friction stir welding tool has a
square pin profile along its axis with flat shoulder profile. The pulsating stir action of
square pin profile was observed to increase the plasticized material but in the case of
cylindrical, tapered and threaded pin profiles the pulsating action was absent. The
dimensions and nomenclature of the fabricated tool was shown in the Figure 3.9 Tool
 28
rotational speed, welding speed, and axial force were the process parameters which
were analysed and their influence on mechanical properties were studied in this work.

Figure 3.9 Friction stir welding tool nomenclature

 29
EXPERIMENTAL SETUP

The special purpose machine indigenously fabricated by M/s. R. V.

Machine Tools, Coimbatore, India, was used to carry out friction stir welding
process. The experimental setup employed in this work for conducting the friction
stir welding on Al 6063, Silicon carbide and boron carbide was shown in Figure
3.10.

Figure 3.10 FSW experimental setup

 30
Hydraulic controls are incorporated in the machine to control the friction
stir welding process . The variable speed motor drive was used to vary the spindle
speed in the wide range between 50 rpm to 4000 rpm, displayed on the digital
indicator. The friction stir welding tool was plunged into the work piece using
downward force which creates the frictional heat between the rotating welding tool
and the work pieces. The axial downward force was exerted by the tool head along
with the spindle can be varied in the range between 2 kN to 50 kN. Horizontal table
(700 mm x 350 mm) was used to hold the work pieces, consists of two axis
movements, along length wise (X-axis) and crosswise (Y-axis). The specially
designed fixture was attached to the top of the table to hold the work pieces firmly
during the welding process.

Experimental procedure

The plates of size 100 mm x 100 mm x 10 mm were obtained from the

fabricated stir cast rectangular plate. The fabricated stir cast plates were first cut into
6 mm thick plate by slicing them using a power hacksaw machine. Then the plates
were cut to the required size (100 mm x 50 mm x 6 mm – Based on the literature
survey) using a milling machine was shown in figure 3.11. Burrs were removed, and
edges were prepared flat using grinding and emery polishing process. Before
carrying out the friction stir welding, the specimens were cleaned to avoid any
surface contaminations.

To fabricate square friction stir welding butt joints using single pass, the
test plates were positioned and rigidly clamped to the backing plate using mechanical
clamps as shown in the Figure 3.12 which prevents the plates from lifting during
welding. The backing plate was clamped to the machine bed. A non-consumable
square profiled tool was then rotated clockwise and slowly plunged into the faying
surfaces of the positioned test plates until the welding tool shoulder contacts the
upper surface of the plates.
 31

Figure 3.11 Plates prepared for friction stir welding from stir casting (100 mm
X 50 mm X 6 mm size)

Figure 3.12 Test plated clamped to the backing plate during friction stir
welding process

A short dwell time was allowed for the rotating tool to generate frictional
heat for preheating and to initiating the plastic flow of the material along the joint
line. After that, a vertical downward force was applied on the tool shoulder and then
 32
the weld traverse started. The direction of the welding was perpendicular to the
rolling direction. The plasticized material was transferred from the leading edge of
the tool to the rear side. The tool was traversed along the joint line until it reached the
end of the weld. The rotating tool upon reaching the end of the weld was retracted
from the plate, leaving a key hole at the end of the weld. Figure 3.13 shows the
schematic diagram of the friction stir welding specimen. The typical friction stir
welded plate and samples of friction stir welded butt joint plates were shown in the
Figure 4.6 and 4.7 respectively.

Figure 3.13 Schematic diagram of the friction stir welding Joint.

 33

RS AS

RS – Retreating sideAS – Advancing side

Figure 3.14 Typical friction stir welded plate

Figure 3.15 Samples of friction stir welded butt joint plates

 34
Identifying the Range of Friction Stir Welding Process Parameters

Initial friction stir welding trials were conducted by varying the process
parameters ie, the tool rotation speed, welding speed and axial force. Friction stir
welding trail runs were carried out on 6 mm thick stir cast Al 6063 hybrid composite
to find out the range of friction stir welding process parameters. The process
parameters listed as shown in Table 3.4. Based on the literature survey used in this
study.

Table 3.4 The friction stir welding process parameters

S.No Process Parameter Range

1. Tool Rotational speed (rpm) 800,900,1000,1100 and 1200
2. Welding speed (mm/min) 30
3. Axial force (kN) 10

Specimen preparation and testing

Microstructure Analysis

To reveal the microstructure of material, the samples from the welded

joint was used to prepare the specimen. The specimen were prepared by passing
through a sequence of operations like sectioning, grinding, polishing and etching.
First, the specimen was cut by band saw in the traverse direction. Care must be taken
that the cut samples contains different regions like stir zone, thermo mechanical
affected zone, heat affected zone and base metal. The specimen were ground to make
the edges smoother by a grinding machine and then polished on a polishing wheel
using a sequence of silicon carbide paper of finer grades, to remove the scratches and
abrasions to obtain a mirror-like finish in the specimen. To enhance the
microstructure appearance clearly, the samples were etched after polishing, which
gives a clear image of the size of the grains. The specimens were etched using
Keller’s reagent which was prepared by adding 2.5 percent of Nitric acid, 1.5 percent
of Hydrochloric acid into 95 percent of distilled water by volume. The etched
specimen were washed thoroughly and dried by an electric dryer. Metallographic
 35
study along the various zones of the friction stir welded specimen was carried out by
using a metallurgical microscope and a scanning electron microscope .

Ultimate Tensile Strength

Tensile test is the most common test used to measure the material’s
strength and is an acceptance test for the specification of materials. In this study,
tensile tests were used to assess the strength of the specimen. The Figure 3.16 shows
the dimension of the tensile specimens prepared from the friction stir welded stir cast
Al 6063 hybrid composite as per the ASTM E8M 04 standard. The Figure 3.17
shows the extraction of tensile specimen from the friction stir welded component.
The Figure 3.18 shows the universal testing machine, The Figure 3.19 shows the
specimens prepared from the friction stir welded Al 6063 hybrid composite. The
tensile test was carried out by gripping the specimen and increasing pull was applied
using a computerized control and then the ultimate tensile strength were estimated.
Three specimen were tested for the purpose of repeatability, and the average value of
ultimate tensile strength was considered for the analysis.

All dimensions are in mm

Figure 3.16 Dimension of tensile specimen

 36

Figure 3.17 Extraction of tensile specimen from friction stir welded joints

Figure 3.18 Universal testing machine.

 37

Figure 3.19 Tensile specimen prepared from friction stir welded joints

Micro Hardness

The micro hardness test is mostly used for small parts, thin sections, etc.,.
To evaluate the hardness of the welded specimen, the following procedure was
employed for the preparation of the specimen. The specimen were prepared the
dimensions as shown in the Figure 3.20 using standard metallurgical procedures and
were etched to perform micro hardness tests at different locations such as stir zone,
thermo mechanical affected zone, heat affected zone and base metal..

All dimensions are in mm.

Figure 3.20 Dimensions of macro/microstructure and microhardness
specimen.
 38
The experimental setup, the procedure involved and fabrication of
friction stir welding of Al 6063 hybrid composite have been explained in this
chapter. Trial runs were conducted to find out the range of the friction stir welding
process parameters. Specimen were prepared and tested as per the standard procedure
which we been explained in this chapter.
 39

CHAPTER 4

RESULTS AND VALIDATION

Introduction

This chapter presents the general microstructure of friction stir welding,

effect of friction stir welding process parameters on the microstructural modification,
and the mechanical properties of friction stir welded stir cast Al 6063 hybrid metal
matrix composites. Even though, the published literature on the effect of tool rotation
speed on mechanical and metallurgical properties of friction stir welding joints for Al
alloys are significant in numbers, the reported information on the effect of tool
rotation speed for Al 6063 hybrid metal matrix composite is very limited. Hence, in
this investigation an attempt was made to understand the effect of tool rotation speed
and its subsequent influence on tensile strength, micro hardness and microstructure
of friction stir welded Al 6063 hybrid metal matrix composites.

Experimental Work

Five joints were fabricated from each Al 6063 hybrid metal matrix
composites and in total fifteen joints were fabricated by varying the tool rotation
speed and keeping welding speed and axial force constant. Trial experiments were
carried out to find out the working limits of tool rotation speed and then the joints
were visually inspected for external weld defects. The tool rotation speeds, which
produced welds of good appearance, were identified to fabricate the joints. The
parameters used to fabricate the joints are presented in Table 4.1. The welded joints
were sliced using power hacksaw and then machined to the required dimensions to
prepare tensile, micro hardness and micro/macrostructure specimens.
 40

Table 4.4 FSW process parameters used to fabricate the joints

Tool rotation speed Welding speed Axial force (kN) Heat input*
(rpm) (mm/min) KJ/mm
800 30 10 1.20638
900 30 10 1.35716
1000 30 10 1.50795
1100 30 10 1.65875
1200 30 10 1.80955

* Heat input was calculated using the following expression

(Heurtier et al 2006, Lakshminarayanan et al 2007).

q = (2π/3S) µ F N R η (5.1)
q = Heat input (kJ/mm)
S= Welding speed (mm/min) F= Axial force (kN)
N= Tool rotation speed (rpm) R= Tool pin radius (m)
µ = Coefficient of friction η = Welding efficiency

From the Table 5.1, it can be inferred that the heat input is having directly
proportional relationship with tool rotation speed. If the tool rotation speed increases,
heat input increases correspondingly.

Results

Macrostructure

All the fabricated joints were analyzed at low magnification (10X) using
optical microscope to reveal the quality of weld region. The macrostructure and
observations made from the macrostructure of the friction stir welded joints of Al
6063 hybrid metal matrix composites are presented in Tables 4.2, respectively. The
joints fabricated at tool rotation speeds of 800 rpm and 1200 rpm contain tunnel
 41
defect at the retreating side of the weld region. The joints fabricated using tool
rotation 900 rpm, 1000 rpm and 1100 rpm are found to be free from macro level
defects in Al 6063 hybrid metal matrix composites (Table 4.2).

Table 4.5 Effect of tool rotation speed on macrostructure of Al 6063

HMMC joints

Tool Macrostructure Fracture location Remarks

rotation RS AS RS AS
speed(rpm)
800  Tunnel defect at the
retreating side and advanced
side Insufficient heat
generation
900  No defect Sufficient heat
generation

1000  No defect Sufficient heat

generation

1100  No defect Sufficient

stirring

1200  Tunnel defect at the

retreating side Abnormal
stirring of the plasticized
metal

Microstructure

The microstructure of weld region of the defect free joints was analysed
using optical microscopy (OM) and scanning electron microscopy (SEM) are
displayed in Figures 4.5. From the micrographs, it can be inferred that the weld
region of all the joints invariably contain uniformly distributed. However, the size of
the particles is different and it is found to be influenced by the tool rotation speed.
The weld region of Al 6063 hybrid metal matrix composites fabricate during a tool
rotation speed of 1000 rpm shows very fine silicon carbide and boron carbide
particles compared to other joints (Figures 4.5 a &b).
 42
Microstructure Analysis

A typical macrograph of a friction stir welded Al 6063 HMMC joint

containing 10% B4C and 10 % SiC (welded at a tool rotational speed of 1000 rpm,
welding speed 30 mm/min axial force of 10 KN is presented in Figure 5.1. It
consists of three zones, the nugget zone (NZ), the thermo mechanically affected zone
(TMAZ) and heat affected zone (HAZ). It is clearly evident that the shape of the
grain structure in nugget zone is different from the other zones. No major variation is
observed between base metal and HAZ in the macroscopic study.

Figure 4.11 Macrostructure of FS Welded Al 6063-10 %B4C-10% SiC

HMMC

The optical micrographs obtained from different zones of welded

composites joined are presented in Figure 4.5 SEM photomicrographs of NZ of FS
welded HMMCs are also presented. The etchant used reveals B 4C particles in white
and Si C in black color.

Tensile Strength

The effect of the tool rotational speed on the tensile strength of friction
stir welded stir cast Al 6063 hybrid metal matrix composites is shown in the Figure
4.2. From the figure, the following inferences were obtained. Friction stir welding
joints were fabricated by using the above said tool rotational speeds by keeping the
other friction stir welding parameters constant. The joint fabricated at a tool
rotational speed of 1000 rpm yielded higher tensile strength. The friction stir welding
joint fabricated at a lower tool rotational speed of 800 rpm have exhibited lower
tensile strength. When the tool rotational speed was increased from 800 rpm, the
 43
UTS of the friction stir welding joints also increases correspondingly. The UTS of
the friction stir welding joints reaches maximum at 1000 rpm. If the tool rotational
speed was further increased beyond 1000 rpm, the UTS of the friction stir welding
joints gets decreased.

Lower tool rotational speed of 800 rpm generates insufficient heat input,
results in the lack of stirring leads to pinhole or tunnel defects in the stir zone was
revealed in the macrostructure observations as shown in the Table 4.2, was the main
cause for the inferior tensile strength. When the tool rotational speed increases from
800 rpm to 1000 rpm, the UTS of the friction stir welding joints increases from the
lower strength value and reaches maximum strength value before falling again at
higher tool rotational speed. This increase in the tensile strength was due to the
increase in the heat input in the stir zone, because of higher frictional heat generation
results in intense stirring, uniform distribution of fine grained silicon particles and
mixing of materials in the stir zone. At higher tool rotational speed beyond 1000 rpm
the strength starts to reduce, was due to the higher heat generation leads to the release
of excessively stirred material to the upper surface which results in producing micro
voids in the stir zone. The yield strength variation of the samples under different tool
rotational speed was shown in the Figure 4.3 The yield strength pattern of friction stir
welded stir cast aluminium alloy hybrid metal matrix composites was similar to that
of tensile strength, although with different varying values. The causes for the
increase in yield strength were similar to that for an increase in tensile strength.
 44

Al 6063 HMMC
200

180 181.5
UTS (Mpa)

160
154.2

140 142.9
131.5
124.1
120

100
700 800 900 1000 1100 1200 1300
Tool Rotational Speed (RPM)

Figure 4.12 Effect of tool rotation speed on tensile strength of Al 6063 hybrid
metal matrix composites

Al 6063 HMMC
200

180
Yield Strength ( Mpa)

170.6
160

140 140.2
130.1
125.5
120 120.4

100
700 800 900 1000 1100 1200 1300
Tool Rotational Speed (RPM)

Figure 4.13 Effect of tool rotation speed on yield strength of Al 6063 hybrid
metal matrix composites
 45
Microhardness

The hardness measurements were performed with 1 mm spacing across

the weld. Fig 4.4 shows the hardness profiles of friction stir welded hybrid metal
matrix composites. It is found that the considerable increase in hardness was
observed in the weld zone when compared to the base metal. Mainly thermal
exposure during the friction stir welding governs the hardness of the joints. Hardness
drop was resulted in the TMAZ, and HAZ was due to the annealing process. From
Fig.4.4 it is found that the maximum microhardness of 105.5Hv was observed at the
stir zone. From the centre of the bead, the hardness is decreased gradually with
increasing distance from the stir zone. The same trend is observed in all the cases of
hardness profiles shown in the figure 4.4. The maximum microhardness of 105.5 Hv
was observed at 1000 rpm. The hardness of the SZ was found to be in the range of
95 Hv to 105.5 Hv which was higher than the base metal hardness. Increase in the
tool rotational speed from 800 rpm increases the microhardness value from 92 Hv.
The maximum microhardness value of 105.5 Hv was recorded for the joint made
using the tool rotational speed of 1000 rpm. Increasing the tool rotational speed from
1000 mm/min reduces the microhardness value. The measured hardness values are in
agreement with the tensile strength results and SZ grain size. The joints with
maximum weld region hardness exhibited higher tensile strength than the other
joints.
 46

Effect of tool rotation speed Al 6063 HMMC 800 RPM

109 900 RPM

106 1000 RPM

103 1100 RPM

Microhardness (Hv)

100 1200 RPM

97
94
91
88
85
5 3 1 -9 -7 -5 -3 -1 1 3 5 7 9 11 13 15
-1 -1 -1
Distance from weldcentre (mm)

Figure 4.14 Effect of tool rotation speed on microhardness of weld zone

The weld region of the Al 6063 hybrid metal matrix composites,

fabricated using a tool rotation speed of 1000 rpm reveals finer particles compared to
their counter parts (Figures 4.5 a&b). The presence of very fine and uniformly
distributed particles in the weld region may also be one of the reasons for higher
tensile strength of these respective joints.
 47
Optical Micrograph

a) 1000rpm
SEM Micrograph
(b)1000rpm
Figure 5.15
Effect
of tool

rotation speed on weld region microstructure of Al 6063 hybrid metal matrix

composites.

1.1 DISCUSSION
 48
The five tool rotation speeds used to fabricate Al 6063 hybrid metal
matrix composites, the joint fabricated at a tool rotation speed of 1000 rpm yielded
higher tensile strength. The joints fabricated using the tool rotation speeds lower and
higher than these values, exhibited comparatively lower tensile strength.
Macrostructure observations (Tables 4.2) showed that the joints fabricated at higher
tool rotation speeds (1200 rpm ) contained tunnel like defects in the weld region and
resulted in lower tensile strength. As tool rotation speed increased resulting inferior
tensile strength due to rise in temperature, which increases the coarsening of SiC and
B4C particles.

Moreover a higher rotational speed causes excessive release of stirred

materials to the upper surface, which resultantly left voids in the weld zone.. On the
other side, the area of the weld zone decreases with decreasing the tool rotation speed
and affect the temperature distribution in the weld zone. The hardness value in the
weld nugget of Al 6063 hybrid metal matrix composites was found to be higher than
that of the base metal, The variation in microhardness of the joints (Figure 4.4) is due
to changes in the heat input caused by frictional heat produced by rotating tool and
subsequent alterations in the microstructure. When the spindle speed is increased, the
hardness values initially rise and converge at higher spindle speeds. This behavior
corresponds to the development of a more uniform temperature distribution within
the weld region as the heat input is increased. It is also noticeable that the hardness
value starts to decrease again at higher rotational speeds. The hardness of the stir
zone decreases with increasing rotational speed. In the stirred zone higher
temperatures are reached than in the HAZ during welding. Thus in the stir zone the
precipitates coarsened even start to dissolve. The number of particles in the stir zone
is lower than that in the parent material. The temperature reached in friction stir
welding is much below the melting point, but is sufficient enough to induce
dissolution or over aging of precipitates. Moreover, at high rotational speeds,
particles would suffer more fragmentations. Thus, these segregated particles are
more likely exist within other parts of the TMAZ. The microstructural variations
affected the mechanical properties within and adjacent to the weld zone
 49
If tool rotation speed increases, the stirring action and heat input are also
increased, thus the size of the silicon carbide and boron carbide particles are reduced
and resulted in the increase of hardness and strength. The fineness and the dispersion
of silicon carbide and boron carbide particles mainly depend on the tool rotation
speed which in turn decides strength of the joints. The tensile properties and fracture
locations of the joints are to a large extent, dependent on the tool rotation speed and
other welding parameters. If the joints are associated with defects like pinhole, tunnel
and cracks in the weld region, the joints failed at the defective area. If the joints are
defect free, the failure locations shifted towards retreating side.

The effect of tool rotation speed on tensile strength, macrostructure, microhardness

and microstructure of friction stir welded Al 6063 hybrid metal matrix composites
was analysed in detail. In this investigation, a tool rotation speed of 1000 rpm for Al
6063 hybrid metal matrix composites are found to be optimum to get maximum
tensile strength of friction stir welding joints. Defect free weld region with very fine,
uniformly distributed Silicon carbide and boron carbide particles are the reasons for
higher hardness and superior tensile strength of these joints.
 50

CHAPTER 5

CONCLUSION
This chapter presents the details of the conclusions from the present
research work which involved the fabrication of Al 6063-SiC- B 4C hybrid
metal matrix composites through stir casting process and the joining of hybrid
metal matrix composites by FSW. The scope for future work is also detailed.

PRACTICAL IMPLICATION OF THIS RESEARCH

The implication of this research is as follows:

The optimized friction stir welding process parameter is very much

useful in producing defect free joints in ship building, aerospace, automobile field
and marine applications.

As 100 % joint efficiency is obtained in the friction stir welding welds, it

contributes 30 % reduction in weight in ship building and marine application. The
advantages of weight reduction in marine vessels increases the payload and
decreased power consumption.

The optimized process parameters hold an entry in the manufacturing

data book of Naval Research Board.

PROJECT CONTRIBUTIONS

The aluminium 6063 hybrid metal matrix composites reinforced with 5%,
10% and 15 % weight of SiC and constant weight of 10 % B 4C were fabricated by
stir casting route. The optical and SEM metallographic studies revealed the presence
of SiC and B4C particles in the HMMCs dispersed homogenously in the matrix. The
incorporation of SiC and B4C with molten aluminium was enhanced due to the
addition of K2TiF6 flux during mixing. The microhardness of the composites where
increased from 82 Hv to 93 Hv with respect to addition of weight % of SiC particles.
 51
The additions of reinforcements into the matrix enhances the tensile strength from
205.6 M Pa to 225MPa. (As per table 3.3, Fig 3.7 and 3.8).

The sound Al 6063 HMMCs were friction stir welded successfully.

Friction stir welding joints were fabricated by varying the process parameters like
Tool Rotation Speed (TRS), Welding Speed (WS) and Axial Force (AF). The
mechanical property such as tensile strength and microstructure were evaluated to
understand the influence of various friction stir welding process parameters.

The microstructure showed that at low tool rotation speed of 800 rpm
produces insufficient heat which intern results in coarse grain size. The increase of
tool rotation speed generates sufficient heat results in fine grain size. The tool
rotation speed 1000 pm results in fine grain size further increase in the tool rotation
speed results in coarse grain size due to increasing heat input.

The highest UTS for the welded composite plates was obtained with the
parameter setting: TRS - 1000 rpm, WS 30 mm/min and AF 10 kN.

SCOPE FOR FUTURE WORK

 Finite element method could be used to detail out the temperature and stress
distribution on the weldments by varying process parameters and reinforcements.

 Dissimilar FSW of hybrid MMCs with the alloys or other HMMCs can be carried
out by varying the friction stir welding process parameters to investigate the
mechanical and metallurgical properties.

 Wear testing, corrosion testing, impact testing, fracture toughness testing and
thermal stress analysis are the potential areas to be explored in depth.

 Study on mechanical and metallurgical properties of post heat treatment of

friction stir welded aluminium matrix hybrid composite can be taken for further
scope of work.
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LIMITATION OF THE RESEARCH

The limitation of this research is as follows:

 The optimized process parameter is applicable only for square tool.

 As the tool is stationary and the table of the machine is moving, the butt joints
can be welded.

 In present work, FSW is carried out for the butt joint configuration and same can
be further extended to other weld joint configurations

 Experiments can be attempted with thicker materials with different tool

geometries and tool angles which have not been considered for the present work.
 53

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