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CHAPTER 3

MATERIALS AND METHODS

3.1

INTRODUCTION

Based on the literature survey and research objectives discussed in

have been developed. A description of the procedure for alloy and composite

production various test procedures adopted to evaluate the properties of

composites are discussed in this chapter. Design of Experiments approach

used and optimisation techniques employed are presented in this section.

Modelling techniques used are also explained in detail.

3.2

PLAN OF INVESTIGATIONS

The plan of investigations is shown in Figure (3.1). Important

of composites, identification of manufacturing process of composites, design

of experiments techniques and studies on mechanical properties (ultimate

tensile strength,

abrasive

following headings.

the

36

37

3.3

MATERIALS

In the present study, composites have been developed to evaluate

reinforcements for composite preparation used are discussed in the following

sections.

3.3.1

Matrix material

The desirable properties required for aluminium alloy matrices are

stability, high compression and tensile strength and economic efficiency. In

the present study, Al-Si10Mg was used as the matrix material. Al-Si10Mg

alloy exhibits excellent resistance to corrosion under both ordinary

atmospheric and marine conditions along with high strength and hardness.

The chemical composition of this alloy is given in Table 3.1.

Table 3.1Chemical composition of Al-Si10Mg matrix alloy (in weight %)

Others

Mg

Si

Fe

Mn

3.3.2

Cu,Ni,Zn,Pb,Sn

andTi

Al

1.5 max

Balance

Reinforcements

Reinforcement is the material, which is added to improve the

hard reinforcement such as Al2O3, SiC strengthens the matrix both

extrinsically, through improved load transfer intrinsically by increasing the

dislocation density. Soft reinforcement like graphite and molybdenum

38

disulphide (MoS2) contribute to lowering wear rate, friction and increasing

seizure resistance.

In the present study, both hard and soft reinforcement has been

used to produce composites. SiCp reinforcement with an average particle size

of 40 m with a density of 3210 kg/m3 was used to produce the composite.

The melting point of the SiC is 2890 C, has a very low reactivity in molten

metal and is relatively cheap. A significant enhancement in composite

properties, such as stiffness, strength and fracture toughness, as well as low

reactivity and the low cost make this reinforcement ideal for the manufacture

of cast metal matrix composites requiring very good wear resistance.

Molybdenum disulphide, a solid lubricant has been used as a soft

reinforcement in this research. The average particle size of MoS2 used was

1.5 m and has a density of 4800 kg/m3. Lubrication effectiveness /efficiency

of MoS2 often exceeds that of graphite and are effective in a vacuum where

graphite fails. However, the efficiency of MoS2 lubrication decreases after

675 K wherein it begins to form MoO3, which lowers the lubricating effect.

MoS2p have superior load bearing and surface speed performance values in

comparison to either graphite or tungsten disulphide.

3.4

The Al-Si10Mg alloy was charged into an electrical resistance-

melting process was carried out at 1073 K under argon atmosphere in a

graphite crucible. Mixing of reinforcement was conducted using a stainless

steel impeller. Schematic diagram of the stir casting setup is shown in

Figure 3.2. Calculated quantity of reinforcement pre-heated at 600K was

added to the molten metal slowly with continuous stirring. Stirring was

continued for a further period of ten minutes after adding the reinforcement.

39

The molten mixture was solidified in a cast iron die in the form of cylindrical

pin of a diameter of 15 mm and length of 75 mm. In the present work, AlSi10Mg MMCs reinforced with 10 wt. % and 20 wt. % SiCp were produced.

The same procedure was repeated for to produce AMCs reinforced with 2 wt.

% and 4 wt. % MoS2p. Hybrid metal matrix composite with 2 wt. % and 4 wt.

% of MoS2p and with 10 wt. % and 20 wt. % SiCp were also cast. As cast

composites and machined wear pin, samples shown in Figure 3.3.

40

3.5

MICROSTRUCTURAL CHARACTERISATION

Microstructural characterisation of the composite specimens was

carried out using Carl Zeiss Goettingen Optical microscope. The specimens

were metallographically polished as per standards to obtain average

roughness value of 0.8 m. The specimens were etched with 2% hydrofluoric

acid. Optical micrographs of the polished specimens were recorded at

different magnifications.

3.6

Properties of the composites as well as matrix alloy specimens

specimens prepared were machined using a CNC machine to a dimensional

tolerance of 0.1mm. Equipments used for testing along with the test

procedures are described in the following sections.

41

3.6.1

Density measurement

Density of composites as well as matrix alloy was determined using

Archimedean principle, a solid body immersed in a liquid apparently loses as

much of its own weight of the liquid it has displaced. The density of the solid

body was determined by using a liquid of known density (Water). Standard

cylindrical specimens of 14mm diameter and 20mm length were used for

these tests. Average readings of three random specimens for each

composition were taken as the density of the composite specimen.

3.6.2

Micro hardness values of the composites as well as matrix alloy

with a diamond indenter. The test surface was prepared to obtain a

metallographic finish; 50-gram load was employed with a dwell time 15

seconds for each sample. An average of five readings taken at different

locations was taken as the hardness of composite specimen.

3.6.3

Tensile testing was carried out as per ASTM E8 using a

Figure 3.4.

42

3.6.4

Morphology studies

Morphology of fractured surface as well as the worn surface of the

composite specimen for tensile test was carried out using JEOL JSM 6360,

T100 Scanning Electron Microscope (SEM). Surface morphology was studied

different magnifications.

3.6.5

A Pin-on-Disk apparatus was used for dry sliding wear tests,

conducted as per ASTM G-99 standard. Initial and final weight of the

specimen was measured using a Mitutoyo make electronic weighing machine

with an accuracy of 0.0001 g. Wear tests were conducted on 10 mm diameter

and 25 mm long cylindrical specimens against a rotating EN-32 steel disc

(counter face) having a hardness 65 Rc. The difference in weights before and

43

after the test was taken as weight loss. Each test was repeated three times and

the results were averaged. Wear Rate (WR) of the composites was studied as

a function of sliding velocity, applied load and sliding distance. WR was

calculated based on the difference in weights of the specimen using the

Equation (3.1) for a constant sliding distance of 3000m.

[

]=

(3.1)

= Density of the material in kg/mm3

D = sliding distance in m

Figure 3.5

this study

44

Table 3.2 Specifications of the Tribo-system

Make

Testing Standard

: ASTM G99

Pin size

: 3 12 mm

Disc size

: 100 mm x 8 mm thick

Sliding velocity

: 0.26 10 m/s

: 200 N

Frictional force

: 0 200 N

3.6.6

The same pin-on-disc type apparatus was employed to evaluate the

conducted on cylindrical specimens of 10mm diameter and 30mm length. The

disc was covered with a commercial SiC emery sheet bonded to the rotating

disc. In order to allow exposure of fresh abrasive material, the specimen was

moved against the parallel surface of the rotating steel disc. Mass loss of the

specimens was measured before and after the wear test using an electronic

weighing balance (accuracy 0.0001 g). Experiments were repeated thrice with

additional specimens to obtain sufficient data for significant results. WR was

calculated based on the difference in weights of the specimen using the

Equation(3.1) for a constant sliding distance of 100m.

45

3.7

INTEGRATED

RESPONSE

SURFACEGENETIC

BEHAVIOUR OF COMPOSITION

RSM is defined as the statistical tool that uses quantitative data

from appropriate experimental design to determine and simultaneously solve

multivariate equations. Genetic Algorithm (GA) is direct, parallel, stochastic

method for global search and optimisation, which mimic the evolution of

humans. In order to combine the benefits of both RSM and Genetic algorithm

an integrated RSM GA approach was adopted. RSM-GA approach used for

modelling, analysing and optimising the materials propertied has been

outlined in Figure 3.6.

Determination of Variables, which

affect material properties

Design of Experiments

Measurement of the Material Property

Development of Response Surface Model(s) (RSM)

Analysis of Variance (ANOVA)

Formulation of Fitness function from RSM

Optimization using Genetic Algorithm

Confirmation Experiment(s)

46

RSM-GA is a blend of experimental design, statistical method and

optimisation technique for constructing an empirical model and for achieving

optimum conditions. The procedure for RSM-GA is shown below

Step 1:

and levels at which they are to be examined.

Step 2:

Box-Behnken Design)

a. Central Composite Design (CCD)

Central composite designs are often recommended when the

design plan calls for sequential experimentation because these

designs can incorporate information from a properly planned

factorial experiment. This design can handle effectively two

factor experiments.

b. Box-Behnken Design

Box-Behnken designs are used when performing non-sequential

experiments. That is, when planning to perform the experiment

just once. These designs allow efficient estimation of the firstand second-order coefficients. Since Box-Behnken designs have

fewer design points, they are less time to run than Central

Composite designs with the same number of factors. BoxBehnken designs also ensure that not all factors are set at their

highest levels simultaneously. A comparison of CCD and Box

Behnken design are shown schematically in Figure 3.7.

47

a) Central Composite Design b) Box-Behnken Design

Step 3:

Step 4:

By conducting experiments and applying regression analysis, a

model of the response to a number of independent input variables

can be achieved. From the model of the response, a near optimal

point can then be obtained. RSM has been frequently useful in the

modelling and optimisation of processes. If X1, X2, ...,Xn are n

number of independent variables and y is a dependant variable

based on the independent variable, then y is called the response .

The observed response, y, can then be written as a function of the

various

independent

Y=f(X1,X2,...,Xn) +

variables,

where

X1,X2,...,Xn

as

follows.

response surface, is obtained. The form of f(X1,X2,...,Xn)

is

approximating

f(X1,X2,...,Xn)

by

suitable

lower-ordered

48

The aim of using RSM is not only to examine the response over the

whole factor space, but also to find the region of importance where

the response attains its optimum or near optimal value. By carefully

examining the response surface model, the combination of factors,

which offer the best response, can then be determined. The values

of the regression coefficients of the linear, square and interaction

terms of the RSM models can be determined by using the relation.

B (X T X ) 1 X TY

(3.2)

calculation matrix X and Y is the matrix of measured response

under study. Coefficient of determination (R 2) is used to test the

goodness-of-fit of the developed mathematical model and provides

a measure of variability in the observed response values. It can be

explained by the controllable factors and their interactions.

Predicted RSM WR was compared with the corresponding

experimental values .The error percentage is given by

Average

Error %

100

n

n

i 1

Y Exp i Y Pr ed

Y Exp i

(3.3)

the Y (Pred)i is predicted response by RSM model corresponding to

ith trial

Step 5:

ANOVA was first evolved by Sir Ronald Fisher (a British

Statistician) is a method of partitioning variability into identifiable

sources of variation and the associated degrees of freedom in a

49

given experiment. The F-test is simply a ratio of sample variances.

Comparing the F-ratio of a source with the tabulated F-ratio is

called the F-test. When Analysis of Variance has been performed

on a set of data and the respective sums of squares have been

calculated, it is possible to use this information to distribute the

corrected sums of squares to the appropriate factors. Comparing

this value with the total sum of squares, gives the percent of the

contributions of each factor can be obtained. The percent

contribution due to error provides an estimate of the adequacy of

the experiment. Since error refers to unknown effects and which

cannot be controlling factors, the percent contribution due to error

suggests that if the sufficiency due to error is low (15% or less),

then it can be assumed that no important factors have been omitted

from the experiment.

Step 6:

Contour and surface plots are useful for establishing desirable

response values and operating conditions. A contour plot provides a

two-dimensional view where all points that have the same response

are connected to produce contour lines of constant responses.

A surface plot provides a three-dimensional view that may provide

a clear picture of the response surface.

Step 7:

Genetic Algorithm (GA) is a direct, parallel, stochastic method for

global search and optimisation, which mimic the evolution of

humans. GA is becoming increasingly popular in the optimization

i.e. maximization or minimization of a resultant response based on

process conditions. The GA sequence in this work is shown in

Figure 3.8

50

The concepts of GA are directly derived from natural evolution and

are based on the mechanics of natural selection and natural

genetics. Basic Steps in Genetic algorithm are

(i)

Coding Structure

The primary step in GA is to decide the coding structure. A set of

coding structure is termed as a chromosome. Each individual

chromosome is usually described as a string of symbols from

(0,1) which are labelled as Genes. The number of bits that must

be used to describe the parameters is problem dependent. Let

each solution in the population of N such solutions Xi, i=1, 2, .. .,

N, be a string of symbols (0,1) of length L. The length of L is

determined by the number of variables affecting the optimum

solution. The relationship between phenotype and genotype of

individual chromosome is shown in Figure 3.9.

51

(ii) Create Initial Population

Typically, the initial population of N solutions is selected

completely at random, with each bit of each solution having a

50% chance of taking the value 0. The jth gene of ith individual

chromosome can be denoted in matrix form as Xij. Population

(POP) = ( Xij) where i=1, 2, .. ., N ; j = 1, 2, .. ., L The genetic

algorithm requires a fitness function. The fitness of an individual

chromosome in a genetic algorithm is the value of an objective

function for its phenotype.

(iii) Evaluating the fitness

For calculating fitness, the chromosome has to be first decoded

and the objective function has to be evaluated. The fitness not

only indicates how good the solution is, but also corresponds to

how close the chromosome is to the optimal one. The best

mathematical model obtained from RSM in coded form used as

the fitness function for the model. The selection of the

chromosomes to produce successive generations are important in

Genetic Algorithm. Several selection schemes such as Roulette

52

wheel, Uniform selection and Tournament selection are available.

Among them Roulette wheel selection is one of the most widely

used scheme in the selection process. It is a probabilistic selection

method, which is based on the individuals fitness such that the

better individuals have an increased chance of being selected. In

this scheme, parent selection is based on roulette wheel where

each member of the population is represented by a slice whose

size is decided by members fitness. A selection step is then a

spin of the wheel, which in the long run tends to eliminate the

least fit population members. The probability P, for the individual

selection is defined by :

P[X isc hosen] =

)

)

>0

(3.4)

(iv) Reproduction

Reproduction options control how the Genetic Algorithm creates

the next generation. The reproduction options used by the GA are

Elite chromosome, Cross over chromosome and Mutation

Chromosome. The reproduction consists of basically three steps.

a. Selection

Elite Chromosomes are specified by the number of individuals

with the best fitness values namely Elite Count (Ne) in the current

generation, which are guaranteed to survive to the next

generation. The Elite Chromosome fraction of the next generation

population (N) is

P =

(3.5)

53

Setting Ne to a high value causes the fittest individuals to

dominate the population, which can make the search less

effective. Besides Elite Chromosome, GA uses the individuals in

the current generation to create the children that make up the next

generation namely, Cross over Chromosome and Mutation

Chromosome. Crossover takes genes from a pair of individual

chromosome (parents) in the current generation and combines

them to form a pair of children (Cross over Chromosome 1 and

Cross over Chromosome 2).

b. Crossover

The number of Cross over Chromosome in the next generation is

termed as Cross over Count (Nc). Crossover fraction is Pc which

ranges from 0 to 1. A random number R is generated and

compared with the probability parameter Pc. If the random

number is less than Pc, a crossover operation is selected,

otherwise, no crossover is performed and the individual parent is

returned. If the crossover operation is selected, then a random

number called the crossover point Rc is generated between 1 and

length of the chromosome Lc.

functions are available like one point crossover, the two point

cross over and heuristic cross over and so on . One-point

crossover is one of the popular crossover methods wherein a pair

of children chromosome is formed by interchanging the last Lc

Rc elements of the first parent chromosome and last Lc

elements of the second parent chromosome.

Rc

54

c. Mutation

Mutation applies random changes to the genes of individual

chromosome (parent) in the current generation to produce a single

new individual child. The number of Mutation Chromosome in

the next generation is termed as Mutation Count (Nm). Mutation

is performed by using techniques like Binary, uniform, Gaussian

as well as adaptive algorithms. The uniform Mutation algorithm

is much suitable in problems like minimisation .It first selects a

fraction of the elements of an individual chromosome for

mutation, where each entry has the same probability as the

mutation rate of being mutated. In the second step, mutation

operator replaces each selected entry by a uniform random

number selected uniformly from user-specified upper and lower

bounds for that element.

type of children in the next generation are as follows: Elite count

Ne= E; Cross over count Nc = (N-E)* Pc; Mutation count Nm =

N-(Ne+Nc).

(v) Decoding

On achieving optimisation, the best chromosomes are decoded

into required factor value.

55

3.8

SUMMARY

Wear processes in composites are a difficult phenomenon

wear characteristics of the composites are affected by these parameters.

Selecting the correct operating conditions is always a major concern as

traditional experiment design, would require many experimental runs to

achieve a satisfactory result. In any process, the desired testing parameters are

either determined based on experience or by use of a data book and do not

provide optimal testing parameters for a particular situation. An approach

based on DoE technique was adopted to obtain maximum possible

information with a minimum number of experiments. Genetic Algorithm was

used to obtain optimum conditions for wear testing.

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