Ti-3Al-2.

5V COMPOSITE REINFORCE
WITH WC AND CHARACTERIZE ITS
EFFECT:METALLURGIAL AND
CORROSION

19MEPN6601-INNOVATIVE AND CREATIVE PROJECT

Submitted by

DHIANESHWAR.K (19BME001)

DARSHAN.S.P (19BME009)

RESHMAA.S.V (19BME013)

in partial fulfillment for the award of the degree

of
Bachelor of Engineering

im

Mechanical Engineering

Dr. Mahalingam College of Engineering and Technology

Pollachi - 642003
An Autonomous Institution
Affiliated to Anna University, Chennai - 600 025
JUNE 2022
 Dr. Mahalingam College of Engineering and Technology
Pollachi - 642003
An Autonomous Institution
Affiliated to Anna University, Chennai - 600 025

BONAFIDE CERTIFICATE

Certified that this project report, “ Ti-3Al-2.5V Composite Reinforced with WC

and Characterize its Effect: Metallurgical and Corrosion” is the bonafide work of

DHIANESHWAR.K (19BME001)

DARSHAN.S.P (19BME009)

RESHMAA.S.V (19BME013)

Who carried out the project work under my supervision.

SIGNATURE OF HOD SIGNATURE OF SUPERVISOR

Dr. I. RAJENDRAN M.E., Ph.D., FIE, Dr. T. RAMKUMAR. M.E., Ph.D.,

Senior Professor &
Head of the Department
Mechanical Engineering
Dr. Mahalingam College of Engineering and
Technology, NPT-MCET Campus
Pollachi – 642003 India
Assistant Professor (S.G.)
Mechanical Engineering
Dr. Mahalingam College of Engineering
and Technology, NPT-MCET Campus
Pollachi – 642003 India

Submitted for the Autonomous End Semester Examination Project viva-voce held on
.

INTERNAL EXAMINER EXTERNAL EXAMINER

 ACKNOWLEDGEMENT
We wish to acknowledge with thanks for excellent encouragement given by the
management of our college and we thank Dr. C. Ramaswamy, M.E., Ph.D., FIV,
Secretary, NIA Educational Institutions for providing us with a plethora of facilities in
the campus to complete our project successfully.

We wish to thank our Principal Dr. A. Rathinavelu, M.Tech., Ph.D., for his
motivation.

We express our extreme gratefulness to Dr. I. Rajendran, M.E., Ph.D., FIE,

Head of the Department, Mechanical Engineering who was instrumental in providing
such wonderful support, which any student would dream to have.

It is also our primary duty to thank our Project guide Dr. T. Ramkumar,
M.E., Ph.D., Assistant Professor (S.G.), Mechanical Engineering, who is back bone of
all our project activities, for his constant guidance and encouragement, which kept us
fast and pro-active in our work. It is their enthusiasm and patience that have borne
fruit in the end.

Finally, we wish to express our deepest gratitude and indebtedness to our

parents for their kind support.
 Ti-3Al-2.5V COMPOSITE REINFORCED WITH WC
AND CHARACTERIZE ITS EFFECT:
METALLURICAL AND CORROSION

ABSTRACT
Titanium alloys are used in airframe structures, landing gear components, and jet engine parts
for their unique combination of properties: moderate density, high strengths, long fatigue life,
fracture toughness, creep strength, and excellent resistance to corrosion and oxidation. The aim
of this project is to develop a material with less weight and more wear resistance and analyze
the suitability of the developed materials for aerospace applications. Composite specimens
are fabricated using Microwave Sintering technique considering Titanium as matrix
and WC as particulate Micro hardness of Ti-WC composites are determined. Wear
tests are conducted using Pin on Disc apparatus for Ti-WC composite specimens.
Wear rate for different loads and speeds are analyzed. The morphology structure of Ti-
WC composites are analyzed before and after wear test using SEM studies. Composition
Ti-WC composite specimens are verified using EDAX analysis. The corrosion behavior of
Ti-WC composite specimens are investigated using TAFEL exploration and SEM analysis.
The developed Titanium-based composite materials have less weight, more wear and
corrosion resistance. Hence, these composite materials are better applicant materials for the
Aerospace applications.

Keywords: Ti-3Al-2.5V, WC, Microstructure, EDAX, Wear, TAFEL

i
 TABLE OF CONTENTS

ABSTRACT ......................................................................................................................................i

TABLE OF CONTENTS ................................................................................................................. ii

LIST OF FIGURES ........................................................................................................................ iii

LIST OF TABLES. .......................................................................................................................... iv

1. INTRODUCTION… ..................................................................................................... 1
1.1 Composite Materials… ................................................................................................. 2
1.1.1 Polymer Matrix Composites… ................................................................................ 2
1.1.2 Metal Matrix Composites… .................................................................................... 3
1.1.3 Ceramic Matrix Composites… ................................................................................ 3
2. LITERATURE REVIEW .............................................................................................. 5
2.1 Objectives… ................................................................................................................. 8
3. METHADOLOGY ........................................................................................................ 9
3.1 Powder Metallurgy ....................................................................................................... 9
3.2 Selection of Composites ............................................................................................. 10
3.3 Sintering ..................................................................................................................... 11
3.3.1 Advantages of Sintering ........................................................................................... 12
3.4 Microstructure............................................................................................................ 13
3.4.1 Scanning Electron Microscope .............................................................................. 13
3.5 Energy Dispersive X-ray Analysis .............................................................................. 16
3.6 X-Ray Power Diffraction ............................................................................................ 17
3.7 Wear Test… ............................................................................................................... 19
3.7.1 Pin On Disc ............................................................................................................ 19
4. RESULTS AND DISCUSSION .................................................................................. 22
4.1 Wear Rate… ............................................................................................................... 22
4.2 Co-Efficient Of Friction .............................................................................................23
4.3 Porosity and Relative Density..................................................................................... 24
4.4 TAFEL Graph… ......................................................................................................... 25
4.5 SEM Results .............................................................................................................. 26
4.6 EDAX Mapping of SEM Images… ........................................................................... 29
5. CONCLUSION .......................................................................................................... 31
6. REFERENCES ............................................................................................................ 32
ii
 LIST OF FIGURES
Figure 1 Powder Metallurgy Process… ............................................................................. 9
Figure 2 Photographic image of Sintering Furnace ........................................................... 11
Figure.3 Photographic image of SEM… ........................................................................... 13

Figure 4 X -Ray Diffraction…...........................................................................................18

Figure 5 Sample XRD Graph…......................................................................................... 19
Figure 6 Pin on Disc Apparatus… ..................................................................................... 20
Figure 7 Schematic Diagram of Pin on Disc… ................................................................. 21

Figure 8 Wear rate of the Composites with Respect to Load (N) ....................................22
Figure 9 Wear rate of the Composites with Respect to Sliding

Velocity (SV) ...................................................................................................22

Figure 10 Friction Co-Efficient of the Composites With respect to

Load (N) ...........................................................................................................23

Figure 11 Friction Co-Efficient of the Composites With respect to

Sliding Velocity (m/s) ..................................................................................... 23

Figure 12 Porosity and Relative Density Graph .............................................................. 24

Figure 13 TAFEL Graph of the Composite Samples ...................................................... 25

Figure 14 SEM Image of the Pure Ti Grade 9 Alloy ..................................................... 26
Figure 15 SEM Image of Ti-3Al-2.5V+0.5 WC Alloy ................................................... 27
Figure 16 SEM Image of Ti-3Al-2.5V+ 1 WC Alloy ...................................................... 27
Figure 17 SEM Image of Ti-3Al-2.5V+1.5 WC Alloy .................................................... 28

Figure 18 SEM Image of Ti-3Al-2.5V+ 2 WC Alloy ...................................................... 28

Figure 19 EDAX Mapping of Pure Titanium Grade 9 alloy after
Corrosion Test… ........................................................................................... 29

Figure 20 EDAX Mapping of Titanium Grade 9 alloy Reinforced with

WC after Corrosion Test ............................................................................... 30

iii
 LIST OF TABLES
Table I Chemical Composition of Ti Grade 9 .................................................................. 10

Table II Corrosion rate of the Composite Sample........................................................................ 26

iv
 LIST OF ABBREVIATIONS

EDS/EDX - Energy Dispersive X-Ray Spectroscopy

FIB - Focused Ion Beam

MMC - Metal Matrix Composite

MMCp - Particulate Metallic Matrix Composite

SEM - Scanning Electron Microscope

TEM - Transmission Electron Microscopy

EDAX - Energy Dispersive X-ray Analysis

FF - Friction Factor

WR - Wear Rate

WL - Wear loss

v
1. INTRODUCTION

Ti-3Al-2.5V (Grade 9) is a near α-type titanium alloy. The composition is Ti-

3Al-2.5V. It is processed to cold - processed tubes. Its strength is 20% - 50% higher
than that of pure titanium at room temperature and high temperature. It has excellent
welding property and cold forming performance. TA18 alloy is generally used in the
condition of annealing. It can be used in cold processing and stress annealing. The
maximum working temperature is about 315 ˚C. TA18 seamless tube is suitable for
the aircraft, engine hydraulic and fuel oil pipeline system. It can be rolled into
titanium foils and titanium strips which are mostly used in honeycomb structure of
aircrafts.
Grade 9 (Ti-3Al-2.5V) alloy is an alpha-beta alloy that has improved strength
over commercially pure titanium grades. This grade also has excellent corrosion
resistance, formability and weldability.

Titanium Grade 9 is much stronger than commercially pure titanium because

of its mechanical properties. Titanium Grade 9 can be cold worked because of its 3%
Aluminium and 2.5% Vanadium, giving it excellent resistance to corrosion,
moderately high strength and good ductility.

Grade 9 when manufacturing, labor and production costs are considered

despite bring alpha-beta titanium alloys with 90% of their alloy composition in
common.

Titanium Grade 9 is superior metals with corrosion-resistant characteristics

and excellent strength. Titanium 3-2.5 alloy can easily meet needed component
specifications can definitely negatively impact the bottom line.

Ti Grade 9 (Ti-3Al-2.5V) is a titanium grade characterized by excellent

corrosion resistance to seawater and higher mechanical properties than stainless steels.
The Ti-3Al-2.5V alloy is characterized by: Excellent resistance to general corrosion –
High mechanical strength, superior strength to weight ratio – Resistant to stress
corrosion – Excellent resistance to pitting, crevice, and erosion corrosion – Good
formability and weldability – Very low thermal expansion – Excellent fatigue
properties.

1
1.1 Composite Materials

A Composite material is a material made from two or more constituent

materials with significantly different physical or chemical properties that, when
combined, produce a material with characteristics different from the individual
components.

The composite materials are commonly classified based on matrix constituent.

The major composite classes include:

 Polymer Matrix Composites (PMC),

 Metal Matrix Composites (MMC) and

 Ceramic Matrix Composites (CMC).

1.1.1 Polymer Matrix Composites (PMC)

Polymers make ideal materials as they can be processed easily, possess

lightweight, and desirable mechanical properties. It follows, therefore, that high
temperature resins are extensively used in aeronautical applications. Two main kinds
of polymers are thermosets and thermoplastics. Thermosets have qualities such as a
well-bonded three-dimensional molecular structure after curing.

They decompose instead of melting on hardening. Merely changing the basic

composition of the resin is enough to alter the conditions suitably for curing and
determine its other characteristics. They can be retained in a partially cured condition
too over prolonged periods of time, rendering Thermosets very flexible. Thus, they
are most suited as matrix bases for advanced conditions fiber reinforced composites.
Thermosets find wide ranging applications in the chopped fiber composites form
particularly when a premixed or moulding compound with fibers of specific quality
and aspect ratio happens to be starting material as in epoxy, polymer and phenolic
polyamide resins.

Thermoplastics have one- or two-dimensional molecular structure and they

tend to at an elevated temperature and show exaggerated melting point. Another
advantage is that the process of softening at elevated temperatures can reversed to

2
regain its properties during cooling, facilitating applications of conventional compress
techniques to mould the compounds.

1.1.2 Metal Matrix Composites (MMC)

Metal matrix composites, at present though generating a wide interest in

research fraternity, are not as widely in use as their plastic counterparts. High
strength, fracture toughness and stiffness are offered by metal matrices than those
offered by their polymer counterparts. They can withstand elevated temperature in
corrosive environment than polymer composites. Most metals and alloys could be
used as matrices and they require reinforcement materials which need to be stable
over a range of temperature and non-reactive too. However, the guiding aspect for the
choice depends essentially on the matrix material. Light metals form the matrix for
temperature application and the reinforcements in addition to the aforementioned
reasons are characterized by high moduli.

Most metals and alloys make good matrices. However, practically, the choices
for low temperature applications are not many. Only light metals are responsive, with
their low density proving an advantage. Titanium, Aluminium and magnesium are the
popular matrix metals currently in vogue, which are particularly useful for aircraft
applications. If metallic matrix materials have to offer high strength, they require high
modulus reinforcements. The strength-to weight ratios of resulting composites can be
higher than most alloys. The melting point, physical and mechanical properties of the
composite at various temperatures determine the service temperature of composites.
Most metals, ceramics and compounds can be used with matrices of low melting point
alloys. The choice of reinforcements becomes more stunted with increase in the
melting temperature of matrix materials.

1.1.3 Ceramic Matrix Composites (CMC)

Ceramics can be described as solid materials which exhibit very strong ionic
bonding in general and in few cases covalent bonding. High melting points, good
corrosion resistance, stability at elevated temperatures and high compressive strength,
render ceramic-based matrix materials a favourite for applications requiring a
structural material that doesn’t give way at temperatures above 1500ºC. Naturally,
ceramic matrices are the obvious choice for high temperature applications. High
modulus of elasticity and low tensile strain, which most ceramics possess, has
3
combined to cause the failure of attempts to add reinforcements to obtain strength
improvement. This is because at the stress levels at which ceramics rupture, there is
insufficient elongation of the matrix which keeps composite from transferring an
effective quantum of load to the reinforcement and the composite may fail unless the
percentage of fiber volume is high enough. A material is reinforcement to utilize the
higher tensile strength of the fiber, to produce an increase in load bearing capacity of
the matrix. Addition of high-strength fiber to a weaker ceramic has not always been
successful and often the resultant composite has proved to be weaker.

When ceramics have a higher thermal expansion coefficient than

reinforcement materials, the resultant composite is unlikely to have a superior level of
strength. In that case, the composite will develop strength within ceramic at the time
of cooling resulting in micro cracks extending from fiber to fiber within the matrix.
Micro cracking can result in a composite with tensile strength lower than that of the
matrix.

4
2. LITERATURE REVIEW

S. Gollapudi et al. (2008) [1] has discussed the creep mechanisms were elucidated
in the light of standard creep models supported by the substructures studied by
transmission electron microscopy. Microstructural observations along with
parametric variations of creep rates were useful in identifying the underlying
deformation mechanisms.

E.M. Ruiz-Navas etal. (2012) [2] has discussed that Ti-3Al-2.5V powders
produced by the blending elemental or the master alloy addition approaches are
suitable for obtaining almost fully dense materials whenprocessed by vacuum hot-
pressing

L. Bolzoni et al. (2012) [3] has discussed the Mechanical properties such as
hardness and flexural strength similar to those of the respective wrought materials
are easily obtained

P.G. Esteban et al. (2012) [4] has discussed the Various relative densities between
83% and 95% pore structures and grain sizes can be obtained by selecting a proper
sintering temperature, but when thealloying elements have to diffuse to homogenise
the composition, a minimum temperature of 1100 1C should be selected

L. Bolzoni et al. (2013) [5] has discussed the ductility is lowered due to the residual
porosity and the relatively high amount interstitials dissolved. Moreover, thermal
conductivity and electrical resistivity values similar to those of the wrought alloy by
processing the Ti-3Al-2.5V alloy by means of pressing and sintering

Kopac J et al. (2013) [6] has discussed the Liquid or gas nitrogen has been able to
decrease the friction coefficient and material transfer when Ti6Al4V and uncoated
carbide pins were used, while a significant improvement has been noted for
Inconel718 and TiN coated pins.

5
 E. Gordo et al. (2014) [7] has discussed the Higher hardness and ultimate tensile
strength can easily be obtained whereas care must be taken to keep high ductility

Anil K et al. (2014) [8] has discussed the experimental results of a recent study on
built-up welded beams are presented in this paper with the primary objective of
enabling design, facilitating fabrication, and implementation of large structural
members forpotential applications in the structural and defense-industry.

Juanjuan Qi et al. (2020) [9] has discussed the Friction and wear tests were
conducted under both room and elevated temperature. Mg MMCs exhibited
outstanding anti-wear and self-lubricating properties in addition to enhanced
mechanical strength.

F.V. Vodolazskiy et al. (2020) [10] has discussed the increase in total content of
alloying elements in investigated alloys contributes to decrease of CTE value as
well as to raise of volume effect of polymorphic transformation upon heating to the
temperature range of occurring of α + β→ β- transformation.

F. Yang et al. (2020) [11] has discussed that it is found that high relative density
values and chemical homogeneity are achieved regardless of the sintering technique
or chemistry of the alloy. Both wrought-equivalent and low-cost Fe-bearing powder
metallurgy Ti alloys were analyzed.

M., Gupta et al. (2021) [12] has discussed that this is a high strength alloy, which
leads to large values of cutting force, a low thermal conductivity causes the
appearance of high cutting temperatures. Dry machining is very useful for
sustainability and clean manufacturing, as it has minimal environmental impact

Sharma S et al. (2021) [13] has discussed the mechanical characteristics like tensile-
strength, flexural-strength, toughness, hardness, scratch adhesion, percent-porosity
and density were studied. A drum type wear apparatus was utilized to evaluate the
6
percentage of wear-loss in different compositions using different loads and it was
found that the wear-loss decreases linearly as the muscovite percentage was
increased.

McDonald A et al. (2021) [14] has discussed the mechanisms contributing to the
material removal and the influence of different parameters on these mechanisms
were evaluated. The effects of the WC particle size and volume fraction on the
scratch depth and worn volume of the composite were also analysed.

7
2.1 Objectives
• To fabricate the titanium grade 9 by reinforcing with WC through powder
metallurgy route.

• To characterize the fabricated composites using Scanning Electron

Microscope and Energy Dispersive Spectroscopy.

• To evaluate the Wear and Corrosion behavior of the composites.

8
3. METHODOLOGY
3.1 Powder Metallurgy
Powder metallurgy is the process of blending fine powdered materials, pressing them
into a desired shape or form (compacting), and then heating the compressed material
in a controlled atmosphere to bond the material (sintering). Figure 1 shows the detail
powder metallurgy process.

• The powder metallurgy process consists of four basic steps:

• Powder manufacture/purchase

• Powder blending.

• Compacting.

• Sintering.

Figure 1 Powder Metallurgy Process

9
3.2 Selection of Composition

• Ti3AI/2.5V alloy is a near alpha, alpha-beta alloy, sometimes referred to as

―half-6-4.‖ It offers 20 to 50% higher tensile strength than the commercially
pure titanium at room and elevated temperatures

• It is used principally as tubing in aircraft hydraulic systems and as foil in

aircraft honeycomb panels. Its applications include aerospace parts, sports
Equipments, medical and dental implants. The chemical composition of
titanium grade 9 is displayed below Table I.

Table I Chemical composition of Ti Grade 9.

Titanium
Balance (92 to 95%)
Aluminum
3
Vanadium
2.5
Iron
≤0.25
Carbon
≤0.05
Hydrogen
≤ 0.015
Oxygen
≤0.12
Nitrogen
≤0.02

Tungsten Carbide

Tungsten carbide is a dense, metal like substance, light gray with a bluish tinge that
decomposes, rather than melts, at 2,600° C (4,700° F). It is prepared by heating
powdered tungsten with carbon black in the presence of hydrogen at 1,400°–1,600° C
(2,550°–2,900° F).

10
Specimen Calculation:
m
�=
�

Where, � - Density, m- Mass and - Volume

3.3 Sintering
Sintering is static when a metal powder under certain external
conditions may exhibit coalescence, and yet reverts to its normal behavior when
such conditions are removed. In most cases, the density of a collection of grains
increases as material flows into voids, causing a decrease in overall volume. Mass
movements that occur during sintering consist of the reduction of total porosity
by repacking, followed by material transport due to evaporation and condensation
from diffusion. In the final stages, metal atoms move along crystal boundaries to
the walls of internal pores, redistributing mass from the internal bulk of the object
and smoothing pore walls. Surface tension is the driving force for this movement.
A typical inert Sintering Oven is shown in Figure 2.

Figure 2 Photographic Image of Sintering Furnace

11
 A special form of sintering (which is still considered part of powder
metallurgy) is liquid-state sintering in which at least one but not all elements are
in a liquid state. Liquid-state sintering is required for making cemented carbide or
tungsten carbide. Sintered bronze in particular is frequently used as a material for
bearings, since its porosity allows lubricants to flow through it or remain captured
within it. Sintered copper may be used as a wicking structure in certain types of
heat pipe construction, where the porosity allows a liquid agent to move through
the porous material via capillary action. For materials that have high melting
points such as molybdenum, tungsten, rhenium, tantalum, osmium and carbon,
sintering is one of the few viable manufacturing processes. In these cases, very low
porosity is desirable and can often be achieved. Sintered metal powder is used to
make frangible shotgun shells called breaching rounds, as used by military and
SWAT teams to quickly force entry into a locked room. These shotgun shells are
designed to destroy door deadbolts, locks and hinges without risking lives by
ricocheting or by flying on at lethal speed through the door. They work by
destroying the object they hit and then dispersing into a relatively harmless
powder. Sintered bronze and stainless steel are used as filter materials in
applications requiring high temperature resistance while retaining the ability to
regenerate the filter element. For example, sintered stainless steel elements are
employed for filtering steam in food and pharmaceutical applications, and sintered
bronze in aircraft hydraulic systems. The Sintering process is carried out in
Dr.Mahalingam College of Engineering and Technology, Pollachi, Tamil Nadu.

3.3.1 Advantages of Sintering

The use of microwave energy for materials processing has major potential
and real advantages over conventional heating. These include:

 Time and energy savings

 Rapid heating rates

 Considerably reduced processing time and temperature

12
  Fine microstructures and hence improved mechanical properties and better
product performance

 Lower environmental impact

3.4 Microstructure

3.4.1 Scanning Electron Microscope

A scanning electron microscope (SEM) is a type of electron

microscope that produces images of a sample by scanning the surface with a
focused beam of electrons. The electrons interact with atoms in the sample,
producing various signals that contain information about the sample's surface
topography and composition. The electron beam is scanned in a raster scan pattern,
and the beam's position is combined with the detected signal to produce an image.
SEM can achieve resolution better than 1 nanometer. Specimens can be observed
in high vacuum in conventional SEM, or in low vacuum or wet conditions in
variable pressure or environmental SEM and at a wide range of cryogenic or
elevated temperatures with specialized instruments. The Parts of a SEM is shown
in Figure 3.

Figure 3 Photographic Image of Scanning Electron Microscope

The most common SEM mode is detection of secondary electrons emitted

by atoms excited by the electron beam. The number of secondary electrons that
can be detected depends, among other things, on specimen Topography. By
scanning the sample and collecting the secondary electrons that are emitted using
13
a special detector, an image displaying the topography of the surface is created.
The signals used by a scanning electron microscope to produce an image result
from interactions of the electron beam with atoms at various depths within the
sample. Various types of signals are produced including secondary electrons (SE),
reflected or back-scattered electrons (BSE), characteristic X-rays and light
(cathodoluminescence) (CL), absorbed current (specimen current) and transmitted
electrons. Secondary electron detectors are standard equipment in all SEMs, but it
is rare that a single machine would have detectors for all other possible signals.

In secondary electron imaging, or SEI, the secondary electrons are emitted

from very close to the specimen surface. Consequently, SEM can produce very high-
resolution images of a sample surface, revealing details less than 1 nm in size. Back-
scattered electrons (BSE) are beam electrons that are reflected from the sample by
elastic scattering. They emerge from deeper locations within the specimen and
consequently the resolution of BSE images is less than SE images. However, BSE are
often used in analytical SEM along with the spectra made from the characteristic X-
rays, because the intensity of the BSE signal is strongly related to the atomic
number (Z) of the specimen. BSE images can provide information about the
distribution of different elements in the sample. For the same reason, BSE
imaging can image colloidal gold immuno-labels of 5 or 10 nm diameter, which
would otherwise be difficult or impossible to detect in secondary electron images in
biological specimens. Characteristic X-rays are emitted when the electron beam
removes an inner shell electron from the sample, causing a higher- energy electron to
fill the shell and release energy. These characteristic X-rays are used to identify the
composition and measure the abundance of elements in the sample.

Due to the very narrow electron beam, SEM micrographs have a large
depth of field yielding a characteristic three-dimensional appearance useful for
understanding the surface structure of a sample. This is exemplified by the
micrograph of pollen shown above. A wide range of magnifications is possible,
from about 10 times (about equivalent to that of a powerful hand-lens) to more

14
than 500,000 times, about 250 times the magnification limit of the best light
microscopes.

The SEM is taken in PSG College of Engineering and Technology,

Coimbatore, Tamil Nadu.

3.4.1 Sample Preparation

Samples for SEM have to be prepared to withstand the vacuum conditions

and high energy beam of electrons, and have to be of a size that will fit on the
specimen stage. Samples are generally mounted rigidly to a specimen holder or
stub using a conductive adhesive. SEM is used extensively for defect analysis of
semiconductor wafers, and manufacturers make instruments that can examine any
part of a 300 mm semiconductor wafer. Some instruments have chambers that can
tilt an object of that size to 45° and provide continuous 360° rotations.

Nonconductive specimens collect charge when scanned by the electron

beam, and especially in secondary electron imaging mode, this causes scanning
faults and other image artifacts. For conventional imaging in the SEM, specimens
must be electrically conductive, at least at the surface, and electrically grounded
to prevent the accumulation of electrostatic charge. Metal objects require little
special preparation for SEM except for cleaning and conductively mounting to a
specimen stub. Non-conducting materials are usually coated with an ultrathin
coating of electrically conducting material, deposited on the sample either by low-
vacuum sputter coating or by high-vacuum evaporation. Conductive materials in
current use for specimen coating with heavy metals may increase signal/noise ratio
for samples of low atomic number (Z). The improvement arises because secondary
electron emission for High-Z materials is enhanced.

An alternative to coating for some biological samples is to increase the bulk

conductivity of the material by impregnation with osmium using variants of the
OTO staining method (O-osmium tetroxide, T-thiocarbohydrazide, O- osmium). Non-
conducting specimens may be imaged without coating using an environmental SEM
(ESEM) or low-voltage mode of SEM operation. In ESEM instruments the specimen
is placed in a relatively high-pressure chamber and the electron optical column is
differentially pumped to keep vacuum adequately low at the electron gun. The
high-pressure region around the sample in the ESEM neutralizes charge
15
and provides an amplification of the secondary electron signal. Low-voltage SEM
is typically conducted in an FEG-SEM because field emission guns (FEG) are
capable of producing high primary electron brightness and small spot size even at
low accelerating potentials. To prevent charging of non-conductive specimens,
operating conditions must be adjusted such that the incoming beam current is equal
to sum of out coming secondary and backscattered electrons currents a condition
that is more often met at accelerating voltages of 0.3–4 kV. Synthetic replicas can
be made to avoid the use of original samples when they are not suitable or available
for SEM examination due to methodological obstacles or legal issues. This
technique is achieved in two steps:
(1) a mold of the original surface is made using a silicone-based dental elastomer,
and (2) a replica of the original surface is obtained by pouring a synthetic resin
into the mold. Embedding in a resin with further polishing to a mirror-like finish
can be used for both biological and materials specimens when imaging in
backscattered electrons or when doing quantitative X-ray microanalysis.

3.5 Energy Dispersive X-Ray Analysis (EDAX)

Energy Dispersive X-Ray Analysis (EDX), referred to as EDS or EDAX, is an
x-ray technique used to identify the elemental composition of materials. Applications
include materials and product research, troubleshooting, deformulation, and more.

EDX systems are attachments to Electron Microscopy instruments (Scanning

Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM))
instruments where the imaging capability of the microscope identifies the specimen of
interest. The data generated by EDX analysis consist of spectra showing peaks
corresponding to the elements making up the true composition of the sample being
analyzed. Elemental mapping of a sample and image analysis are also possible. In a
multi-technique approach EDX becomes very powerful, particularly in contamination
analysis and industrial forensic science investigations. The technique can be
qualitative, semi-quantitative, and quantitative and also provide spatial distribution of
elements through mapping. The EDX technique is non-destructive and specimens of
interest can be examined in situ with little or no sample preparation. In situations
where combined Microscopy and EDX data acquired are insufficient to identify a

16
specimen, complementary techniques are available, typically Infra-red (FTIR)
Microscopy, RAMAN Microscopy, Nuclear Magnetic Resonance Spectroscopy
(NMR) and Surface Analysis (X-ray photoelectron spectroscopy (XPS) or Time-of-
Flight Secondary Ion Mass Spectrometry (SIMS)).

3.5.1 EDAX analysis applications

 Product deformulation and competitor analysis

 Adhesion, bonding, delamination investigations
 Optical appearance, haze and colour problems
 Disputed claim investigations and expert witness
 Failure investigations, identification of cause
 Catalyst quality, poisoning and elemental distribution
 Product imperfections and defect analysis
 Contamination detection, isolations and identification
 Quality control, raw material and end product
 Filler, pigment, fibre, additive distribution, orientation
 Assessment of plant particulate emissions
 Construction and maintenance monitoring (asbestos)

3.5.2 Benefits from EDAX analysis

 Improved quality control and process optimization.

 Rapid identification of contaminant and source.
 Full control of environmental factors, emissions etc.
 Greater on-site confidence, higher production yield.
 Identifying the source of the problem in process chain.

3.6 X-RAY POWDER DIFFRACTION (XRD)

X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for
phase identification of a crystalline material and can provide information on unit
cell dimensions. The analyzed material is finely ground, homogenized, and average
bulk composition is determined.

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X-ray diffractometers consist of three basic elements: An X-ray tube, a sample holder,
and an X-ray detector. The Rays generated are shown in Figure 4.

Figure 4 X-ray Diffraction

X-rays are generated in a cathode ray tube by heating a filament to produce
electrons, accelerating the electrons toward a target by applying a voltage, and
bombarding the target material with electrons. When electrons have sufficient
energy to dislodge inner shell electrons of the target material, characteristic X-ray
spectra are produced. These spectra consist of several components, the most
common being Kα and Kβ. Kα consists, in part, of Kα1 and Kα2. Kα1 has slightly
shorter wavelength and twice the intensity as Kα2. The specific wavelengths are
characteristic of the target material (Cu, Fe, Mo, Cr). Filtering, by foils or crystal
monochrometers, is required to produce monochromatic X-rays needed for
diffraction. Kα1and Kα2 are sufficiently close in wavelength such that a weighted
average of the two is used. Copper is the most common target material for single-
crystal diffraction, with CuKα radiation = 1.5418Å. These X-rays are collimated
and directed onto the sample. As the sample and detector are rotated, the intensity
of the reflected X-rays is recorded. When the geometry of the incident X-rays
impinging the sample satisfies the Bragg Equation, constructive interference occurs
and a peak in intensity occurs. A detector records and processes this X-ray signal
and converts the signal to a count rate which is then output to a device such as a
printer or computer monitor. The XRD graph in Shown in Figure 5.

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 Figure 5 Sample XRD Graph
The geometry of an X-ray diffractometer is such that the sample rotates in the path
of the collimated X-ray beam at an angle θ while the X-ray detector is mounted on
an arm to collect the diffracted X-rays and rotates at an angle of 2θ. The instrument
used to maintain the angle and rotate the sample is termed a goniometer.
For typical powder patterns, data is collected at 2θ from ~5° to 70°, angles that are
preset in the X-ray scan.
The XRD was taken in Alagappa Chettiar College of Engineering and
Technology, Karaikudi, Tamil Nadu.

3.7 WEAR TEST:

3.7.1 PIN ON DISC (POD)

A pin on disc tribometer consists of a stationary "pin" under an applied load in

contact with a rotating disc. The pin can have any shape to simulate a specific
contact, but spherical tips are often used to simplify the contact geometry.
Coefficient of friction is determined by the ratio of the frictional force to the
loading force on the pin. The pin on disc apparatus is shown in Figure 6.

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 Figure 6 Pin on Disc Apparatus

The amount of wear in any system will, in general, depend upon the number of
system factors such as the applied load, machine characteristics, sliding speed, sliding
distance, the environment, and the material properties. The value of any wear test method
lies in predicting the relative ranking of material combinations. Since the pin-on- disk test
method does not attempt to duplicate all the conditions that may be experienced in service
(for example; lubrication, load, pressure, contact geometry, removal of wear debris, and
presence of corrosive environment), there is no endurance that the test will predict the
wear rate of a given material under conditions differing from those in the test.

Test Specimens, the typical pin specimen is cylindrical or spherical in shape.

Typical cylindrical or spherical pin. F is the normal force on the pin, d is the pin or ball
diameter, D is the disk diameter, R is the wear track radius, and w is the rotation velocity
of the disk. The typical disk specimen diameters range from 30 to 100 mm and have a
thickness in the range of 2 to 10 mm. Surface Finish-A ground surface roughness of 0.8
µm (32 µin.) arithmetic average or less is usually recommended. Rough surfaces make
wear scar measurement difficult. Care must be taken in surface preparation to avoid
subsurface damage that alters the material significantly. Special surface preparation may
be appropriate for some test programs. Schematic Diagram of Pin on Disc is shown in Figure
7.

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 Figure 7 Schematic Diagram of Pin on Disc

The disk was made of EN31 steel with hardness of 62 HRC. The diameter of the
sliding track on the disk surface was 100 mm. The wear tests were performed under dry
sliding conditions with the load (10 N – 25 N), rotational speed (100-200 rpm) and
sliding speed (10 m/s).
Wear rate is calculated by,
Wear rate (mm3/m) = Volume loss /Sliding distance
The wear tests were carried out in Dr. Mahalingam College of Engineering and
Technology, Pollachi, Tamil Nadu.

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 4. RESULTS AND DISCUSSION

4.1 Wear rate

The wear rate of the composite samples are carried out in the Pin on Disc Wear Testing
machine under various loads and sliding velocity is taken and the average is taken for
accuracy. The wear rate results are shown below.

Figure 8 Wear rate of the composites Figure 9 Wear rate of the composites
with respect to load (N) with respect to Sliding velocity (m/s)

The Figure 8 shows the wear rate of the composites with respect to load applied. With
the increase in load from 10 N to 30 N the wear rate of the composites increases. It
also shows that the maximum wear rate was recorded for pure Ti-3Al-2.5V at a load
of 30N and the minimum was recorded for Ti-3Al-2.5V+2WC at a load of 10 N.

The Figure 9 shows the wear rate of the composites with respect to sliding velocity.
The sliding velocity was varied from 5 m/s to 25 m/s. It also shows that the maximum
wear rate was recorded for pure Ti-3Al-2.5V at a sliding velocity of 5m/s and the
minimum was recorded for Ti-3Al-2.5V+2WC at a sliding velocity of 25 m/s.

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 4.2 Co-efficient of friction

The Co-efficient of friction of the composite samples are carried out in the Pin on
Disc Wear Testing machine under various loads and sliding velocity is taken and
the average is taken for accuracy. The wear rate results are shown below.

Figure 10 Friction co-efficient of the Figure 11 Friction co-efficient of the

composites with respect to Composites with respect to Sliding velocity
Load (N) (m/s)

The Figure 10 shows the Friction co-efficient of the composites with respect to Load
(N) applied. With the increase in load from 10 N to 30 N the friction co-efficient of
the composites increases. It also shows that the maximum friction co-efficient was
recorded for pure Ti-3Al-2.5V at a load of 30N and the minimum was recorded for Ti-
3Al-2.5V+2WC at a load of 10 N.

The Figure 11 shows the Friction co-efficient of the composites with respect to
sliding velocity (m/s). With the increase in sliding velocity from the friction co-
efficient of the composites increases. It also shows that the maximum friction co-
efficient was recorded for pure Ti-3Al-2.5V at a sliding velocity of 5 m/s and the
minimum was recorded for Ti-3Al-2.5V+2WC at a sliding velocity of 25 m/s.

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 4.3 Porosity and Relative density

The porosity and Relative density of the composite samples are calculated by
Archimedes Principle. The values are shown in the below.

Figure 12 Porosity and relative density graph

The Figure 12 shows the porosity and relative density graph of the composite samples.
The porosity % of the composite Ti-3Al-2.5V+2WC is minimum and has the value of
0.04%. As well as the composite Ti-3Al-2.5V+2WC has maximum relative density
value of 0.98.

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4.4 TAFEL Graph

The TAFEL graph is drawn the relationship between the current generated from the
electrochemical cell and the potential of the specific metal. The TAFEL graph for the
composite samples is made from the values obtained from the TAFEL experiment and
it is shown in figure 13.

Figure 13 TAFEL graph of the composite samples.

The figure 13 shows that the Ecorr value of the composite Ti-3Al-2.5V+1.5WC is
greater than the other composite samples. The corrosion rate of the composite Ti-
3Al-2.5V+1.5WC is lower when compared to the other composite samples. The
value obtained from the TAFEL exploration is display in Table II.

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 Table II Corrosion rate of the composite samples

SPECIMEN CORROSION
COMPOSITION RATE (mil/year)
Ti-3Al-2.5V(PURE) 3.110e+001

Ti-3Al-2.5V+0.5WC 1.761e+002

Ti-3Al-2.5V+1WC 2.295e+001

Ti-3Al-2.5V+1.5WC 5.384e+001

Ti-3Al-2.5V+2WC 7.374e+001

4.5 SEM Results

Figure 14 SEM image of the pure Ti Grade 9 Alloy.

26
Figure 15 SEM image of Ti-3Al-2.5V+0.5 WC alloy.

Figure 16 SEM image of Ti-3Al-2.5V+ 1 WC alloy.

27
 Figure 17 SEM image of Ti-3Al-2.5V+1.5 WC alloy.

Figure 18 SEM image of Ti-3Al-2.5V+ 2 WC alloy.

The SEM analysis of the surface of the Ti-3Al-2.5 V + WC composites is

shown in above Figures 14-18. Figure 14 shows the SEM image of Ti-3Al-2.5 V
(PURE) material composite and Figure 15-18 shows the SEM image of Ti-3Al-2.5V +
X % WC (X varies from 0.5%, 1%, 1.5%, 2%). Small grooves and pits are also
appeared on its surface. Rough surfaces are seen mostly in Figure 18. The presence of
pores and pits present on the surface affects the properties of the sample.

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 4.6 EDAX Mapping of SEM Samples

Figure 19 EDAX mapping of pure titanium grade 9 alloy after corrosion test.

Element Weight % Atomic % Error

%
CK 1.58 4.32 18.04
OK 22.75 46.72 11.09
Na K 1.52 2.17 16.83
Al K 2.9 3.54 9.23
Si K 1.26 1.47 9.99
Cl K 0.52 0.48 13.95
Ti K 49.28 33.8 1.88
La L 12.42 2.94 6.32
Fe K 7.76 4.57 5.33

Figure 19 shows the composition of the Pure Titanium grade 9 alloy. There is a peak of
titanium in between 4.0 keV to 5.0 keV. There is a peak of Fe in between 6.0 keV to
7.0 keV and between 0.0 keV to 1.1 keV with low intensity. Then the peak of
Aluminium in between 1.0 keV to 2.0 keV with low intensity.

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 Figure 20 EDAX mapping of titanium grade 9 alloy reinforced with WC
after corrosion test

Element Weight % Atomic % Error

%
OK 42.66 68.16 10.47
Al K 4.73 4.48 7.13
Ti K 47.28 25.23 1.66
VK 2.27 1.14 7.08
Fe K 1.77 0.81 11.88
WL 1.28 0.18 55.94

Figure 20 shows the composition of the reinforced Titanium grade 9 alloy with
Tungsten Carbide. There is a peak of titanium in between 4.4 keV to 5.5 keV. There is
a peak of vanadium in between 0.0 keV to 1.1 keV and between 4.4 keV to 5.5 keV
with low intensity. Then the peak of Aluminium in between 1.1 keV to 2.2 keV with
low intensity. There is a peak of W in between 1.3 keV to 2.6 keV and a peak of C in
between 1.1 keV to 2.2 keV with low intensity.

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5. CONCLUSION

The Titanium-based composite materials may be effectively used in the aerospace

industry for disc brake applications due to better wear properties. From the entire studies
of reinforced titanium grade 9 with tungsten carbide composites, the following
conclusions are drawn.

 High density composite specimens are fabricated using Sintering technique

considering titanium grade 9 alloy as matrix and tungsten carbide as
particulate reinforcements.
 Wear rate and Co-efficient of friction of pure titanium grade 9 alloy &
reinforced titanium grade 9 alloy by tungsten carbide composites are
determined by Pin on Disc Wear testing machine and from the results, it is
observed that the minimum wear rate was recorded for Ti-3Al-2.5V+2WC
composite sample.
 The porosity and Relative density of the composite samples are calculated by
Archimedes Principle and from the results, it is observed that the porosity of
the composite Ti-3Al-2.5V+2WC is minimum and has the value of 0.04%.
 The Corrosion behavior of the composite samples are done in TAFEL
Experiment and the TAFEL graph. From the experiment, it is observed that
the corrosion rate of the composite Ti-3Al-2.5V+1.5WC is lower when
compared to the other composite samples.
 The morphology structure of composites pure titanium grade 9 alloy &
reinforced titanium grade 9 alloy are analyzed before and after corrosion test
using SEM studies.
 Composition of composite samples pure titanium grade 9 alloy & reinforced
titanium grade 9 are verified using EDAX Mapping.
From the above findings, it is concluded that the reinforced Titanium grade 9 alloy
composite materials have less wear rate, corrosion resistance and low friction
coefficient. Hence, these composite materials are better applicant materials for the
automotive applications.

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