CHAPTER 1

INTRODUCTION

1.1 History

Titanium has received a lot of attention from researchers recently because it has
excellent mechanical qualities like corrosion resistance, strength, fatigue resistance,
and creep resistance. There are numerous uses for titanium and its alloys in
automobiles, construction, industries, and aerospace engines. In order to enhance the
mechanical properties of titanium metal matrix, researchers are currently working on
adding reinforcements.

According to a recent review, there are roughly four different grades or varieties
of titanium alloys: Ti 6AL-4V, Ti 6AL ELI, Ti 3Al 2.5, and Ti 5Al-2.5Sn. The
titanium alloy Ti-6AL-4V is the most widely used. As a result, it is often referred to as
the titanium alloy "workhorse." It is estimated that it accounts for 50% of all titanium
usage worldwide. Ti-6AL-4V is a preferred material in a number of sectors, including
the medical, marine, aerospace, and chemical processing.

Marine engineering is the next significant industry that uses titanium alloys.
Grade 5 Titanium alloy (Ti-6Al-4V) with Kevlar and carbon fibre are the Metal Matrix
Composites that have been used in marine applications. These composites can also be
used in the marine industry as a hull material for naval warships, in the aerospace
industry, in the defence industry, and for the creation of a variety of structures that call
for high strength and impact bearing capacity. Effective use of these materials in the
aforementioned industries lowers the price and size of the materials while improving
performance in terms of, among other things, strength, corrosion resistance,
weldability, and fabricability. The performance of the vessels in terms of speed and
manoeuvrability is sure to improve due to the low density of the materials used.

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Sandwich panelling with isophthalic resins is to be used for the fabrication of the
composites.

1.1.1 Mechanical Properties of Titanium alloys:

Table 1.1 Mechanical Properties of Titanium alloys of various grades.

Properties Grade Grade Grade Grade

I II III IV

Tensile strength 240 345 450 550

(N/mm2)

Yield strength 170 275 380 483

(N/mm2)
Elongation 24 20 18 15
(%)

EI Modulus 102 102 102 104

(GPa)

Density 4.5 4.5 4.5 4.5

(g/cc)
Brinell Hardness 100 110 150 180
(HB)

Based on the above comparison it is clear that the Titanium alloy Grade I is
having the properties, which is feasible to our process.

1.1.2 Advantages of Titanium:

 Resistance to corrosion. When exposed to air, a thin layer of oxide forms on the
surface of titanium.
 High strength.

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  Low thermal expansion.
 Non-toxic.
 High melting point.
 Excellent fabrication possibilities.

1.1.3 Properties of Titanium :

The term titanium metal matrix composites (Ti-MMCs) refers to composite
materials in which titanium (Ti) serves as the matrix material and is embedded with
additional reinforcing materials. These composites are made to improve titanium's
desirable qualities like low density and corrosion resistance while preserving its
desirable properties like strength, stiffness, and wear resistance.

Although the types of reinforcements used in Ti-MMCs can vary, some typical
options include carbon fibres, ceramic reinforcements made of silicon carbide, boron
carbide, or alumina, or metallic reinforcements made of aluminium, titanium, or
chromium. Usually, these reinforcements are incorporated into the titanium matrix as
fibres, particles, or whiskers.

The mechanical properties of the composite can be significantly enhanced by

the addition of these reinforcing materials. In comparison to pure titanium, Ti-MMCs
have higher strength, stiffness, and hardness, which makes them suitable for uses that
call for materials with high performance and low weight. They are useful in demanding
environments due to their enhanced resistance to wear, fatigue, and creep.

Key industries that use Ti-MMCs include those in the automotive, sporting
goods, and aerospace industries. These composite materials are employed in aerospace
applications to create parts for things like aircraft engine parts, landing gear, and
airframe structures. Because of their high strength-to-weight ratio, Ti-MMCs are used
in brake rotors, suspension systems, and engine parts for automobiles, where they can
improve performance and fuel economy.

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1.1.4 Applications of Ti:
 In Aerospace industry for the manufacturing of airplane bodies, missiles, fan
blades, boosters, engine compartments, jet engine parts, compressors.
 In Marine industry, the manufacturing of plastics, salt refining industry,
concentrators, electric tanks, distillation towers, reactors.
 Used in the manufacturing of tennis rackets, ice skates, hiking sticks, badminton
rackets.
 In Biomedical field, they Titanium is used for devices requiring strength,
elongation, and long-term bone bonding in orthopedics, cardiovascular
medicine, dentistry, etc.
 Titanium is a popular choice for jewelry because it is strong and hypoallergenic.

1.1.5 Properties of Chromium:

A hard, brittle, and shiny metal is chromium. Silver-gray in colour, it can be
highly polished. When heated, it births and turns green chromic oxide instead of
tarnishing in the air. Because chromium is unstable in oxygen, it immediately forms a
thin oxide layer that prevents oxygen from penetrating and shields the metal below.

1.2 Powder metallurgy

Powder metallurgy is the science of creating metal powders and creating
finished/semifinished objects from alloyed powders with or without the addition
of nonmetallic components.
1.2.1 Steps in powder metallurgy

Powder production, Compaction, Sintering, &Secondary operations

1.2.2 Powder production

Raw materials - Powder; Powders can be pure elements, pre-alloyed powders

Methods for making powders – Atomization: Produces powders of both ferrous and
non-ferrous powders like stainless steel, super alloys, Ti alloy powders.

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1.2.3 Reduction of compounds

Production of iron, copper, tungsten, and molybdenum for the production of

copper, iron, and silver powders, Mixers are used to combine powders and additives.
Prior to mixing, lubricants like wax, metallic stearates, graphite, etc. are added to
make it easier to eject the compact and reduce tool wear.

1.2.4 Applications

 The main application of using powder metallurgy is that the composite is

having good damping capacity.
 More over the mechanical properties of the composites created by the powder
metallurgy process will improve.
 The strength of the composites is also well improved when compared to that
of all composites.
 The chemical property of the composites are also well improved when
compared to all other methods.

 So finally we choose powder metallurgy is the best and easy process when
compared to all other process.
1.2.5 Procedure

The following are the process of powder metallurgy and it is briefly

Explained

Fig.1.1 Flow chart of powder metallurgy process

The excellent lightweight, high strength, and corrosion resistance qualities of

titanium make it suitable for marine applications. A hard, brittle, and shiny metal is
chromium. Because it is unstable in oxygen, it immediately forms a thin oxide layer

5
that prevents oxygen from penetrating and shields the metal beneath.

1.2.6 Stage I: Particle size conversion

To prevent the formation of air gaps, also known as porosity, the reinforcement's
size had to be reduced to the nanoscale. The planetary mill was used to convert the
particle sizes while running at a constant speed for the estimated amount of time.

Fig.1.2 Photograph of particle size conversion materials

As depicted in the above figure, steel balls and reinforcement are put in the jar
and then it is placed in the planetary mill. A ball mill is a type of grinder used in
mineral dressing processes, paints, pyrotechnics, ceramics, and selective laser sintering
to grind and blend materials. It operates on the idea of impact, and as the balls fall
from nearly the top of the shell, size reduction is accomplished by impact.

A hollow cylindrical shell rotating about its axis makes up a ball mill. The
shell's axis could be horizontal or at a slight angle to the horizontal. Balls make up
some of its partial filling. The balls, which can be made of steel (chrome steel),

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stainless steel, ceramic, or rubber, are the grinding media. The cylindrical shell's inner
surface is typically lined with an abrasion-resistant substance, like rubber or
manganese steel. Rubber-lined mills suffer less wear. The mill's diameter is roughly
equal to its length.

The mill provides as axial rotation which creates striking contact between steel
ball and reinforcement inside jar. This contact reduces the size of reinforcement after
specified time.

1.2.7 Stage II: Elemental mixture

For further processing, the base metal needed to be combined with the
nanoscale reinforcement. The planetary mill that was used for size conversion was
used for this step. Both powders were weighed in accordance with their composition
before being combined in a mill by axial rotation for a predetermined amount of time.
Similar to the stage before, this one has material requirements. The homogeneous
mixing of powders or various wet components with varying specific weights and
particle sizes is accomplished using a ball mill. In order to avoid cross-contamination
between batches and dusting when mixing powders, the product is mixed in a
removable container.

1.2.8 Stage III: Compaction

It is the process of transforming loose powder into a green compact with precise
dimensions. The tools used are steel dies and punches. The die is created to fit the
required specimen dimension. Die steel, such as EN 24, EN 18, etc., is the material
used for dies most frequently. Usually, compaction is carried out at room temperature.
Between 138 MPa and 827 MPa, or more, is the compaction pressure range.

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 Fig.1.3 Photograph of UTM and compaction die

The die is filled with powder, and load is applied using a punch made
specifically for the size of the specimen. For the purpose of compacting the elemental
mixture, the base metal's maximum load capacity is determined. This compaction
process is completed using a hydraulic press or a universal testing machine. To ensure
it can withstand the load applied by the universal testing machine, the compaction die
was constructed and heat treated for 50RC.

The tensile strength and compressive strength of materials are tested using a
universal testing machine (UTM), also referred to as a universal tester, materials
testing machine, or materials test frame. A tensometer is a former name for a tensile
testing device. The "universal" in the name refers to the fact that it can test a variety of
materials, parts, and structures for tensile and compression in accordance with industry
standards. It can be applied to the process of compaction in addition to strength testing.
The acting load can be calculated using the dial gauge in the UTM as depicted in the
above diagram. In hot compaction, the punch is typically released once load is reached.
However, the load is held for a predetermined amount of time after cold compaction.
However, in cold compaction, once the load has been reached in the metre, it is held
for a predetermined amount of time. This will ensure an evenly distributed load
throughout the specimen's volume.

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1.2.9 Stage IV: Sintering
A powder compact is subjected to a heat treatment process called sintering in
order to give it strength and integrity. The temperature used for sintering is lower than
the melting point of the main component of the powder metal material.

Following compaction, nearby powder particles are held together by cold welds,
giving the compact enough "green strength" to be handled. Diffusion processes result
in the formation and growth of necks at these contact points at sintering temperature.

By carefully selecting and zoning the furnace atmosphere, using an appropriate

temperature profile throughout the furnace, and other techniques, these steps and the
sintering process itself are typically accomplished in a single, continuous furnace. But
for some specimens, the heat treatment process cannot be carried out in an open
environment because it could cause oxidation or damage to the specimen if flammable
metals are used. In this situation, inert gas atmosphere furnaces are typically used
instead of regular furnaces. Here, heat treatment is carried out in a nitrogen-filled
electronic muffle furnace. Due to the fact that a cold-compacted specimen is only
slightly more durable than an ice cube, heat treatment is used to increase the
specimen's hardness. This heat treatment procedure enhances toughness and
machinability in addition to hardness.

9
 Fig.1.4 Photograph of sintering set up

1.2.10 Stage V: Hot extrusion

Extrusion is a process used to create objects of a fixed cross- sectional profile. A

material is pushed through a die of the desired cross-section. The two main advantages
of this process over other manufacturing processes are its ability to create very
complex cross-sections, and to work materials that are brittle, because the material
only encounters compressive and shear stresses. It also forms parts with an excellent
surface finish.

Extrusion is used to tighten up pores and enhance the specimen's grain structure.
Extrusion not only accomplishes that but also enhances mechanical qualities like
hardness, compressive strength, tensile strength, etc.

A tapered die and punch must be made out of die steel, EN 24, EN 18, or any

10
other metal suitable for making dies in order to perform extrusion. While the die is
heated for extrusion, the specimen is heated separately. This is done to prevent the
specimen's heating-induced air reaction. While the die is preheated with a bandwidth
heater made for the die's dimensions, the specimen is heated in a muffle furnace. A 100
tonne hydraulic press is used to carry out this extrusion process.

Fig.1.5 systematic representation of Extrusion set up

Hot extrusion is a hot working process that keeps the material from working
hardening and makes it simpler to push the material through the die because it is
carried out above the material's recrystallization temperature. The majority of hot
extrusions are carried out on presses that have a capacity of between 250 and 12,130
short tonnes (230 to 11,000 metric tonnes). As a result, lubrication is necessary, which
can be either oil or graphite for lower temperature extrusions or glass powder for
higher temperature extrusions. Pressures range from 30 to 700 MPa (4,400 to 101,500
psi), so lubrication is necessary.

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 CHAPTER 2
LITERATURE REVIEW

2.1 Composite in marine application:

 Shaokun Yan [1] et al. studied the passivation and bio fouling of titanium and its
alloys in marine environments. Ti alloys are the best materials for use in
engineering applications involving seawater because of their superior
mechanical strength and chemical stability as well as the possibility of weight
reduction. For instance, they have been utilised in the manufacturing of fasteners
for the maritime industry, hydrocarbon extraction tools for the offshore
petroleum and chemical industry, heat exchangers for desalination facilities, and
cooling systems for seawater-cooled power plants.
 I. Gurrappa [2] had conducted research on the characterization of titanium alloy
Ti-6Al-4V for industrial, marine, and chemical applications. The outcomes
demonstrated that under various environmental circumstances investigated at
both low and higher temperatures, the titanium alloy could form a protective
oxide scale. Correlations were found between the corrosion rate assessments
made in various settings and at various temperatures. According to studies on
pitting corrosion in various environments, the alloy is susceptible to pitting and
crevice corrosion in industrial settings but not in chemical or marine settings at
either temperature.
 Harun Mindivan [3] looked into how particle size affected the mechanical
characteristics of Ti reinforced MMCs. Tensile strength and hardness were
discovered to be significantly increased when compared to conventional MMCs
by optimising the particle size of the reinforcement. According to the study's
findings, regulating the particle size distribution is essential for obtaining
superior mechanical properties.

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  Ali Mazahery [4] et al. focused on the fabrication of Ti reinforced MMCs using
powder metallurgy techniques. The researchers examined the microstructure and
mechanical properties of the composites. The results showed that the
incorporation of Ti reinforcement led to a significant increase in both tensile
strength and hardness compared to the base material.
 Yang Zhou [5] investigated how to fabricate Ti reinforced MMCs using in-situ
reaction synthesis and assessed their tensile and hardness properties. In
comparison to the base material, the results revealed a noticeable improvement
in both tensile strength and hardness. The formation of a homogeneous
microstructure and robust interfacial bonding between the matrix and Ti
reinforcement were credited in the study as the causes of these improvements.

2.2 Reinforced Titanium matrix composites in marine application:

 Hailiang Yu [6] et al. studied on the microstructure and mechanical
characteristics of Al/Ti/Al laminate sheets, and examined the effects of
annealing. Roll bonding and annealing at 873 K for durations of 6 to 168 h were
used to create new tri modal laminate sheets made of TiAl3 particles, coarse-
grained Al, and ultrafine-grained Ti. The Al layer was seen to break up and
disperse in the Al matrix during rolling because it was much thicker than the Ti
layer. Between the layers of Ti and Al, TiAl3 particles emerged during
annealing. The laminate demonstrated the best mechanical properties after a 24-
hour annealing period.
 Shuai Wang [7] et al. concentrated on the layered composites' tensile strength,
which was higher than that of the monolithic Ti alloy but lower than that of the
TiBw/TA15 composite. The layered composites' ability to deform uniformly was
superior to that of the materials used in each layer. The uniform elongation and
ultimate elongation were sacrificed, but increasing the composite layer thickness
increased the tensile strength of layered composites.
 Shan Jiang [8] et al. investigated how the Ti64-ZrB2 composites' room- and

13
 high-temperature strengths increased with the addition of ZrB2, primarily
because the TiBw volume fraction increased. Only a small amount of the
strengthening could be attributed to the Zr solid solution. The ductility of the
composites would, however, be severely reduced by a high Zr concentration.
Although adding too much Zr would worsen the anti-creep properties, Zr solid
solution could significantly improve the composites' creep resistance.
 Xueyan Zeng [9] et al. investigated the dry friction performance of a Y2O3
reinforced Ti/ TiC/ TiB composite and the corrosion behaviour of the composite
in simulated seawater and deduced that the in situ synthesised TiC/ TiB leads to
a decreasing dimension of a phase. A purified interface is introduced after the
grains are further refined with the addition of Y2O3 nanoparticles. The
composite's mechanical performance is enhanced by the mounts of Y2O3
nanoparticles adhering to the reinforcements, which strengthens the interfacial
bonding.
 Shaik Mozammil [10] looked into how Ti fibre reinforcement affected MMC
tensile behaviour and hardness. According to the findings, the addition of Ti
fibres significantly improved both tensile strength and hardness. The high
strength and stiffness of the Ti fibres, which successfully resisted deformation
and improved the composites' overall mechanical properties, were credited by
the study with contributing to this improvement.

Analyzing the above review the possible solution found was powder metallurgy
i.e. compaction followed by heat treatment and then extrusion. The advantages of
taking up this method of production was,

 More specimens can be produced easily.

 The base metal selected here is titaniumm which has its young’s modulus of
102 GPa.

 Complex shapes can be easily fabricated using this process.

14
 CHAPTER 3
EXPERIMENTAL PROCEDURE
3.1 Materials

Titanium powder with a mean particle size of 177 m and a purity level of
>99.995% is provided by S D Fine-Chem Limited and used as the base material. As
reinforcement, Merck Life Science Private Limited's chromium particles with a purity
level of >99.5% and a mean size of 45 m are used.

3.2 Procedure

3.2.1 Particle Size Conversion

Titanium has a particle size of about 45 m, which was reduced to an average
particle size of 30–50 nm using a planetary mill that had a jar with 16 metal balls.

With a planetary mill that included a jar with 16 metal balls for size conversion,
chromium with a particle size of about 45 m was reduced to an average particle size of
30–50 nm.

Fig.3.1 Photograph of Particle size conversion 1

15
 With a break every half-hour to clean the balls and scrape the powder that sticks
to the jar walls in order to prevent stickiness and accumulation, this process took 17
hours at 250 rpm of the ball mill. This is done to ensure that, during mixing, chromium
nanoparticles fill all gaps left by titanium microparticles. This guarantees an even
distribution, which enhances the composition's mechanical properties.

Fig.3.2 Images of Particle size conversion 2

3.2.2 Elemental Mixture of Ti-Cr Powders

In five different ratios, including 96:2:2, 92:4:4, 88:6:6, 84:8:8, and 80:10:10,
chromium was added to titanium metal. For each composition, this blending process
took place in the planetary mill at 200 rpm for 10 minutes. Because a supporting paper
demonstrates that properties change minimally at 3 percent, the percentage begins at
w[9]

. Fig.3.3 Photograph of Elemental mixture 1

16
 Fig.3.4 Photograph of Elemental mixture 2

3.2.3 Cold Compaction

At room temperature, the metals that had been blended were compacted. To
create a cylindrical billet with a 25mm diameter and a 50mm length, 42 grams of
powder were weighed for each sample. A punch was used to apply a load of 30kN to
the compaction die, which was fixed inside of a Universal Testing Machine and filled
with weighed powders.

Fig.3.5 Photograph of Cold compaction setup

17
 This load was maintained at a constant pressure for five minutes in order to
produce a solid specimen. Following each compaction, the compaction die was cleaned
with a solution made from 3 parts distilled water and 1 part acetone. Additionally, each
time before filling the die with powder, the internal walls of the die were coated with
graphite powder to reduce friction and improve the surface finish of the specimen. For
each sample, 10 specimens were compressed and kept in airtight zip covers.

Fig.3.6 Photograph of Cold compaction

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COMPACTING PRESSURE TITANIUM:

𝐶𝑂𝑀𝑃𝐴𝐶𝑇𝐼𝑁𝐺 𝐹𝑂𝑅𝐶𝐸(𝑁)
COMPACTING PRESSURE =
𝐹𝐴𝐶𝐸 𝐴𝑅𝐸𝐴

COMPACTING FORCE = COMPACTING PRESSURE OF TITANIUM * FACE AREA

= 488* π/4 * (25)2 = 52.03 KN

Compacting pressure for titanium is 52.03KN ~ 50KN so 50KN load is acceptable.

WEIGHT CALCULATION:

Volume of the specimen = 𝜋𝑟2h

Specimen height needed (h) = 50mm

Radius of the specimen(r) = 12.5mm

Volume of the specimen = 𝜋 *(12.5)2*(50) = 24543.69 * 10−9𝑚3

Mass of the specimen required = density * volume

Density of Titanium (major composition) = 1740 𝑘𝑔

𝑚3

= 1740 * 24543.69∗ 10−9

Mass of the specimen required = 0.0427kg ~ 43g

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3.2.4 Sintering

Sintering is thermal treatment of fine-grained material at a temperature below

the melting point of the base metal, for the purpose of increasing its grain size and
strength by bonding the particles together. The sintering process is done in two stages.
In stage 1, the compacted specimens were sintered for 4 hours in a muffle furnace at
nitrogen atmosphere to prevent reaction of specimen with air. The sintering process
took place at 600℃ which is 75% of melting point of base metal.

The heat treatment temperature is selected of 75% of melting point of base . This
selection for not exceeding 75% is one supporting paper [18] stated that when

temperature of heat treatment exceeds beyond 600oC for Titanium the results produced

are similar to that of specimen heat treated at 600oC. And henceforth the heat

treatment was fixed at 600oC i.e. 75% of total melting point of base metal. Due to
continuous passing of cool nitrogen air into the furnace, the temperature rise took more
time than normal sintering process. It took 1.5 hours to reach 600℃ from room
temperature and then held at 600℃ for 4 hours. A tray was prepared, and specimens
were arranged in the tray in individual crucible and placed inside the furnace.

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 Fig.3.7 Photograph of Sintering setup

The gas was passed through a ceramic tube at 0.5 to 1 bar pressure into the
chamber. Eight samples were heat treated at a time and took approximately 6
hours for one complete sintering process. The stage 2 sintering process is similar
to stage 1, but the only difference is the heating temperature and time of sintering
was reduced. Sintering was done at 400℃ for 1 hour at same nitrogen atmosphere.
And it took 1 hour to reach 400℃ and the furnace was held at 400℃ for 1 hour.
Similar to stage I, 8 samples were sintered at a time and it took approximately 2.5
hours for one complete sintering process.

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3.2.5 Hot Extrusion

Extrusion process is done to improve the matrix grain growth. An extrusion die
had to be fabricated that supports the dimensions of specimen. The extrusion
temperature range for magnesium is 250℃ to450℃. The die was made as split type for
removing excess powder sediments in die after each extrusion process. The reduction
percentage was 20% in diameter i.e. 25mm diameter was reduced to 20mm through

extrusion. And hence the extrusion ratio is 1.25:1 The taper angle of the die is 14o and
length of taper is 10mm. The specimen and die were pre-heated separately to prevent
reaction of specimen with air during heating.

Fig.3.11 Photograph of Specimen at each stage

The above diagram displays the different views of specimen after completion of
each stage namely compaction, sintering and extrusion.

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3.3 Material Characterization

3.3.1 SEM analysis of powder mixture

This test is conducted to investigate the Cr distribution in titanium metal of the
process of elemental mixture. This analysis was done on powders obtained after
elemental mixture of Ti-Cr in scanning electron microscope (SEM). SEM provides
detailed high resolution images of the sample by rastering a focused electron beam
across the surface and detecting secondary or backscattered electron signal. An
Energy Dispersive X-Ray Analyzer (EDX or EDA) is also used to provide elemental
identification and quantitative compositional information.

Fig.3.12 Image of SEM analysis of powder

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3.3.2 Microstructural characterization

This test is carried out to look into Ti-Cr nanocomposites Cr and grain growth.
In terms of materials science, characterization refers to the broad and all-encompassing
process of probing and measuring a material's structure and properties. Without it, no
scientific understanding of engineering materials could be established. It is a
fundamental procedure in the field of materials science. In a scanning electron
microscope (SEM), this microstructural characterization was carried out on the
polished surfaces of extruded composite samples. Microstructural characterization's
experimental set-up is comparable to powder SEM analysis.

Fig.3.13 Schematic diagram of SEM analysis of extruded specimen

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3.3.3 Density measurements

The Archimedes principle was used to calculate the density of sintered Ti-Cr.
Three measurements of each sample were made to obtain a precise density value. A
liquid with a density of 1 g/cm3 was used: water. Using the Archimedes principle, this
density measurement is performed.

Archimedes' principle states that the upward buoyant force that is exerted on a
body immersed in a fluid, whether fully or partially submerged, is equal to the weight
of the fluid that the body displaces and acts in the upward direction at the center of
mass of the displaced fluid.

Fig.3.14 Schematic diagram of Archimedes principle for density calculation

3.3.4 Microhardness test

The microhardness tests were carried out on flat and polished extruded
specimens using a microhardness tester made by the Wolpert Group and a Vickers
indenter.

25
 In order to measure the hardness more precisely, each sample was measured
three times. The Vickers test is an alternative to the l method for determining a
material's hardness. Since the necessary calculations are independent of the indenter's
size and the indenter can be used for all materials regardless of hardness, the Vickers
test is frequently simpler to use than other hardness tests. The basic idea is to observe a
material's resistance to plastic deformation from a standard source, as with all
commonly used measures of hardness.

Fig.3.15 Photograph of Vickers hardness tester

All metals can be tested using the Vickers test, which also has one of the
broadest scales of any hardness test. The Diamond Pyramid Hardness (DPH) or
Vickers Pyramid Number (HV) is the hardness measurement unit provided by the test.
Although the hardness value can be expressed in Pascal's units, pressure, which also

26
uses the same units, should not be confused with it. Pressure is not what determines the
hardness number because that comes from the load applied to the indentation's surface
area rather than the area normal to the force.

Fig.3.16 Schematic diagram of Vickers hardness concept

3.3.5 Compression test

At room temperature, the compressive characteristics of extruded Ti-Cr samples

were evaluated. A test specimen with dimensions of 12 mm in diameter and 20 mm in
length was employed. To ensure repeatable results, each sample was tested three times.

Fig.3.17 Schematic diagram of Compressive strength tester concept

27
 It is very common to use compression testing to determine a material's
compressive force or crush resistance as well as the material's capacity to recover after
being subjected to a specific compressive force and even held for a predetermined
amount of time. The behaviour of a material under a load is assessed using
compression tests. A material's maximum stress tolerance under a load (either constant
or progressive) over time is calculated.

Fig.3.18 Images of Compressive strength tester

Compression testing is frequently carried out to a rupture or a limit. Depending

on the kind of material being tested, break detection can be specified when a test is run
to a break. Either a load limit or a deflection limit is used when the test is run to its
limit.

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Table3.1 Bill of Materials

SI.No Material Quantity Cost

1 Titanium 500 grams Rs. 2800

2 Chromium 500 grams Rs. 2000

3 Acetone 200 ml Rs. 200

4 Graphite 500 grams Rs. 300

5 Compaction die 1 Rs. 2000

6 Punch & stud for compaction 1 each Rs. 100

7 Dowel pin 2 Rs. 30

8 Zip bag covers 50 Rs. 50

9 Miscellaneous Rs. 2000

Total Rs. 9480

29
 CHAPTER 4

RESULTS AND DISCUSSIONS

4.1 SEM image of powder

SEM analysis was conducted on the elemental mixture of Ti and Cr to confirm

the uniform distribution of Chromium reinforcement over Ti matrix in five different
weight percentages.

Fig.4.1 SEM images that showing distribution of nano-Cr particulates in Ti powder:

(a) Ti-2% Cr (b) Ti 4% Cr (c) Ti -6% Cr (d) Ti -8% Cr and (e) Ti -10%Cr

30
 The properties of the resulting matrix would be significantly improved only if
there is a uniform distribution, as this will cause the bonding to improve by grain
growth. Clean, dry, and outgassing-free samples must be prepared for applications
involving the SEM. Desiccating for two days and depositing a few nanometers of gold
are the rules that must be followed. Wet samples cannot be imaged or measured in
their natural state, but if desired, they can be dropped onto a conducting substrate and
analysed in the SEM after the solvent has evaporated (and dried).

4.2 SEM micrograph

The extruded specimen underwent SEM analysis in order to obtain
micrographic images of each nanocomposites composition. As depicted in Fig.4.2, the
nanocomposites' structure and grain growth steadily improved as more Cr
reinforcement was added. Depositing a few nm of gold is one of the preparation
requirements that must be met before testing.

It is evident that the reinforcement is dispersed evenly throughout the matrix.

The effective strategy used during the fabrication of the nanocomposites is the cause of
the uniform distribution of reinforcement particles. The micrographs made it clear that
the Cr distribution was quite homogeneous. The Titanium matrix's grain growth is
caused by hot extrusion. The density of the developed nanocomposites was measured
using the Archimedes principle, and the micrographs also demonstrated the presence of
minimal porosity in these materials.

31
Fig.4.2 SEM images that showing distribution of nano-Cr particulates in Ti
powder: (a) Ti-2% Cr (b) Ti 4% Cr (c) Ti -6% Cr (d) Ti -8% Cr and (e) Ti -
10%Cr

32
4.3 Density and Porosity

A better bond between Ti-Cr and the use of an appropriate extrusion ratio may
be to blame for the composite material's minimal porosity. The results of density and
porosity measurements conducted on the extruded specimen are shown in Table 4.1.

Table 4.1 Results of density and porosity measurements.

S. No Materials Density Porosity

Theoretical Experimental (%)

ρ (g/cm3) ρ (g/cm3)

1 Ti-2% Cr 1.839 1.837 0.1087

2 Ti 4% Cr 1.938 1.937 0.1012

3 Ti -6% Cr 2.039 2.037 0.1339

4 Ti -8% Cr 2.138 2.136 0.1183

5 Ti -10%Cr 2.239 2.236 0.1589

It is well known that porosity significantly affects the mechanical properties; as

a result, pores must be eliminated through the post-sintering process and extrusion.
When compared to reinforced Titanium [18], the porosity of pure magnesium is
higher; when 4 wt% Cr is added to Ti, the porosity level is low. As the weight
percentage of Cr particulates increased, so did the density of composites. The density
characteristics showed very little oxidation of magnesium and no macro pores. The
equation used to determine experimental density is
ρ = Density,
m = Weight or Mass in Air, m2 = Weight in Water,

V = volume calculated using mass (m-m3).

33
 The density of the object is, ρ = m v.
Porosity P= [(ρtheo– ρexp)/ ρtheo]*100
Where ρtheo = Theoretical density, ρexp = Experimental density

Archimedes’ Principle aids in the determination of density by providing a

convenient and accurate method for determining the volume of an irregularly shaped
object, like a rock. This method is quite commonly used in the construction industry. It is
known also as Hydrostatic Weighing.

4.4 Microhardness
Table 4.2 shows the mechanical characteristics at room temperature. Pure
Titanium is discovered to have a very low hardness, while composite materials exhibit
a higher hardness than pure Titanium. However, the hardness of pure Ti is significantly
increased by the addition of nanoscale Cr particulates. The strengthened effects
brought on by the refined grains may be the cause of the increased hardness of
nanocomposites. Cr particulates' synergistic effect on the magnesium matrix led to
improved hardness values. As the amount of additional Cr reinforcement increased, the
value of microhardness grew steadily. The intended load was 0.1 kg with a dwell time
of 15 s.

Table 4.2 Result of hardness.

S. No Composition Average Hardness in HV

1 Ti-2% Cr 37
2 Ti 4% Cr 40
3 Ti -6% Cr 43.67
4 Ti -8% Cr 44.67
5 Ti -10%Cr 50

34
4.5 Compression test

Compressive strength testing is a mechanical procedure that determines the

maximum compressive load that a material can withstand before breaking. A
compression testing machine uses a gradually applied load to compress the test piece,
which is typically in the shape of a cube, prism, or cylinder. Although brittle materials
like rock, brick, cast iron, and concrete may have high compressive strengths, they
eventually fracture. Concrete has a crushing strength of about 3 tonnes per square inch
(commonly referred to as the cube strength), granite has a crushing strength of 10
tonnes per square inch, and cast iron has a crushing strength ranging from 25 to 60
tonnes per square inch. Used was an intending load of 0.1 kg with a dwell time of 15 s.

The compressive strength of extruded Ti-Cr samples were tested at ambient

temperature. The test specimens of diameter 12 mm of five different compositions
were used. The specimen was subjected to compression test at a ram speed of 3 mm
per min. The test was carried out on five different compositions of Ti-Cr
nanocomposites.

Table 4.3 Result of compressive strength.

S. No Composition Compressive strength in MPa

1 Ti-2% Cr (sample 1) 292

2 Ti 4% Cr (sample 2) 307

3 Ti -6% Cr (sample 3) 312

4 Ti -8% Cr (sample 4) 321

5 Ti -10%Cr (sample 5) 330

35
 compressive strength(MPa)
340
330
330
compressive strength (MPa)

321
320
312
307
310

300
292
290

280

270
(sample 1) (sample 2) (sample 3) (sample 4) (sample 5)

compressive strength

Fig.4.3 Graph correlating compressive strength

MICRO HARDNESS TEST (Hv)

60

50
MICRO HARDNESS TEST (Hv)

40

30

20

10

0
(sample 1) (sample 2) (sample 3) (sample 4) (sample 5)

MICRO HARDNESS TEST

Fig.4.4 Graph correlating Microhardness

36
 The composite samples' differences in compressive strength and microhardness
work well together. Despite the initial variation, compressive strength dramatically
increases at higher weight fractions of reinforcement. This might be as a result of the
constrained grain growth at a higher reinforcement content. Depending on how much
reinforcement is inserted into the matrix, density and hardness rise. This is explained
by factors like the abrasiveness of the reinforcement.

37
 CHAPTER 5

CONCLUSION

Ti-Cr nanocomposites were successfully synthesized through powder

metallurgy method followed by sintering and hot extrusion. The technology
route follows as conversion of macro titanium particles to nanoparticles,
preparing the elemental mixture, compacting the elemental mixtures into
cylindrical specimens, sintering the specimens, extruding the specimens, and
characterizing mechanical properties. Based on microstructural and
mechanical characterization following conclusions can be drawn.

 Powder metallurgy method is an efficient technique to fabricate Ti

based composite since the method prevents oxidation of Ti and less
porosity is achieved.

 SEM image confirms the uniform distribution of Cr over Ti matrix and

thus proves homogeneity of the composite. The composition of 20 %
Cr with Titanium shows better homogeneity.
 Density is observed to be increasing as the weight percentage of
reinforcement increases and porosity is minimum due to the fine
bonding of Ti and Cr in the mixture and hence proves the minimum
oxidation of Mg. The composition Ti-4%Crhas low density when
compared to other compositions.
 Hardness and compressive strength has been considerably improved
due to the synergetic effect of Cr particles as the weight percentage of
Cr increases. Hence the composition Ti -10% Cr has higher hardness
and compressive strength when compared to other compositions. It is
observed that the hardness and compressive strength are directly
proportional to the percentage addition of reinforcement. 

38
5.1 Scope of the Project

 The main purpose for the fabrication of this composite is to replace the
alloying elements of steel, aluminium alloys etc.,
 It has high corrosive resistance and hence it is suitable for automobile
parts.

 It is expected to replace high cost corrosive materials used for multiple

purposes.
 The tensile property of the composite is very high hence it is beneficial
for producing ductile materials.
 The Ultimate tensile strength, Yield strength and elastic modulus of the
composite is well improved, hence it is suitable for producing material of
high stiffness.
 The grain growth of the composites improved, so it is more resistance
to boundary slip, interface slip, twinning, dislocation, thus it is used to
produce damping resistance components.
 Cr does not tarnish in air, when heated it burns and forms the green
chromic oxide. Chromium is unstable in oxygen, it immediately
produces a thin oxide layer that is impermeable to oxygen and protects
the metal below.
 Due the light weight of the Ti metal, the fuel efficiency will be much
better.

39
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