FABRICATION OF MAGNESIUM BASED METAL MATRIX

COMPOSITES BY TWO STEP STIR CASTING AND THEIR

GRINDABILITY STUDIES
by

PONAPPA.K
Department of Mechanical Engineering

Submitted
in fulfillment of the requirements of the degree of Doctor of Philosophy
to the

INDIAN INSTITUTE OF TECHNOLOGY DELHI

NEW DELHI- 110016, INDIA
SEPTEMBER 2012

CERTIFICATE
This is to certify that the thesis entitled, Fabrication of magnesium based metal matrix
composites by two step stir casting and their grindability studies being submitted by
Mr. Ponappa.K to the Indian Institute of Technology Delhi for the award of the degree of
Doctor of Philosophy in Mechanical Engineering is a bonafide record of original research work
carried out by him under our supervision in conformity with the regulations of the institute.

The results presented in this thesis have not been submitted, in part or full, to any other
University or Institute for the award of any degree or diploma.

Dr. S. Aravindan

Prof. P. Venkateswara Rao

Associate Professor

Professor

Mechanical Engineering Department

Mechanical Engineering Department

Indian Institute of Technology Delhi

Indian Institute of Technology Delhi

New Delhi 110016 (INDIA)

New Delhi 110016 (INDIA)

ACKNOWLEDGEMENTS

I earnestly thank my research supervisors Dr.S.Aravindan and Prof.P.Venkateswara Rao,

for all what they had done to bring this work to a fruitful end. Their support during the course
of my doctoral work was overwhelming. Both of my supervisors kept continuously guiding
me in all aspects of research, thus instilling in me a research attitude that would never at all
fade into oblivion. Any amount of gratitude would never match the help and support, I got
out of them.

I wish to express my gratitude to Prof.D.Ravikumar, chairman of SRC, Prof.O.P.Gandhi,

external expert member of SRC and Dr.Sunil Jha, internal expert of SRC, for their valuable
suggestions and encouragement in my research work.

The help extended by technical staff members requires special mention. People at the Central
Workshop, Metrology Lab, Welding Lab, Production Engineering Lab, Machine Tool Lab
and Micro-Nano Manufacturing Lab, particularly Mr. Subhash Chand Sansanwal, Mr.
A.Sivakumar, Mr. Ayodya Prasad, Mr. Tulsi Ram, Mr Duli Chand Meena, Mr.P.S. Negi, Mr.
Prabhakar Biswal , Mr.M.Pandey and Mr.Amit Gupta were very friendly and helpful.

It would not have been possible for me to take up this work, without my friends and
colleagues Dr.M.Uthayakumar, Dr.K.Pannerselvam, Mr.K.Raj Kumar, Mr.Dinesh Setti and
Mr. R.Uma Shankar contributed their mite to make my work successful.

I cant suitably thank my parents, for they are above all that. My father Mr.Sethu
Kannayiram and my mother Mrs.Thennammai, who are still ready to make sacrifices for
my well being. The emotional support provided by them during the difficult periods of this
research is remarkable.

My wife Sathyaruba, and my son A.P.Sarvesh are constantly behind me to focus my

energies in this research work.

I acknowledge the support and encouragement extended by my sisters Mrs.Alagammai

Dhanabalan and Mrs.Santhi Ramasamy & my brother Mr.Arunachalam Senthil Kumaran.
Also I thank all, who from within and without helped me in completing this work.

PONAPPA.K

ii

ABSTRACT

Metal matrix composites, the wonder materials with light weight, high strength to
weight ratio and stiffness properties have come a long way in replacing the conventional
materials. The composite materials find wider applications, owing to the increasing need of
higher strength and lower weight of various functional components in the automobile,
aircraft and electronic industries. However, fabrication and machining of metal matrix
composites into commercial products present challenges because of the difficulty and cost
involved.

High strength steels, aluminum and polymeric composites are already used to reduce
the weight significantly. In order to reduce the weight further, the material scientists from all
over the world are focusing their attention on light weight magnesium and magnesium alloy
matrix composites. Compared to other alternative light weight materials such as aluminium
matrix composites and titanium matrix composites, usage of magnesium results in 20-22%
weight reduction. Energy savings, environmental friendliness and reduced cost are the goals
of industries which can be achieved by way of utilizing the novel composite.

Improper selection of manufacturing process will be severely affecting the physical

and mechanical properties of magnesium alloy composites. Among the variety of
manufacturing processes available for metal matrix composites, stir casting is generally
accepted as a promising route for the commercial production. Its advantages lie in its
simplicity and applicability to large quantity production. To improve the particle distribution

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and to increase the wettability, two step mixing is needed i.e., to heat the slurry to a
temperature above the liquidus and then stirring.

Since magnesium alloy (AZ91D) is not readily available in the market in India, Pure
magnesium blocks (99.95% purity) along with 10 % aluminium, 1%

zinc and 0.4 %

manganese were melted inside a mild steel crucible which was, kept in a microprocessor
controlled electric resistance furnace under inert (Argon) environment to cast AZ91D blocks.
After casting, spectroscopic analysis was carried out on the cast magnesium alloy (AZ91D)
to assure that the alloying elements were within the specified range in ASTM standard B275.
After finalizing the addition of alloying elements, in order to fabricate magnesium alloy
(AZ91D) composites, preliminary casting trials were carried out.

The processing parameters such as stirring speed and pouring temperature were
optimized through these experiments. After finalizing all the parameters, magnesium alloyyttria & magnesium alloy- silicon carbide composites were stir cast. The stir cast magnesium
composites were subjected to heat treatment (T6). The stir cast and heat treated magnesium
alloy based composites were evaluated through metallurgical studies such as micro structural
analysis, elemental analysis, phase analysis & mechanical properties such as hardness, and
the strength.

The addition of reinforcement particle to magnesium alloys significantly improves the

stiffness and strength at room and elevated temperatures. Since the density of most ceramic
reinforcements is higher than magnesium, use of magnesium and magnesium alloys as matrix

iv

materials is particularly beneficial in producing a low weight composite. Compared to other

reinforcement particles SiC and Yttria are thermodynamically stable in magnesium and
magnesium alloy melt. The dispersion of the hard particle (SiC and Yttria) in the composites
drastically blocks the dislocation motions. This increases the yield strength and the modulus
of elasticity with the reduction in its ductility. Smaller size particles of SiC exhibited better
properties than the bigger ones.

There was an considerable increase in porosity with the increase in percentage

volume of reinforcement in both (SiC, yttria) the cases. Hardness, youngs modulus, yield
strength and ultimate tensile strength of composites were observed to be increased with
increasing volume percentage of the reinforcement particles. Solution hardening and artificial
aging (T6) condition exhibited improved mechanical properties than that of as cast condition.
Tensile tested (fractured) surfaces of both the composites (SiC, yttria) revealed particle pull
out, matrix cracks adjacent to particles, occasional dimples and limited amount of material
displacement. This confirms the mixed mode of fracture.

Even though the latest technologies are developed for fabricating near net shape
components, the tolerance and the required surface finish for the industrial components
necessitate the machining process as an unavoidable one. Machinability of metal matrix
composites has received considerable attention because of the presence of hard reinforcement
particle, which leads to rapid tool wear. Widespread of industrial applications of these
materials will not be possible without resolving the machining problems. The properties that
make MMCs appealing for their use created major challenges for machining.

Grinding is particularly needed to acquire high dimensional accuracy and surface

finish. However it is difficult to machine hard ceramic reinforced magnesium alloy matrix
composite, because the reinforcement and matrix of the composite possess widely different
properties. Further, relatively softer magnesium alloys exhibit poor grindability due to
clogging of the wheel by the chip adhesion/ loading, while extremely abrasive hard ceramic
particle can influence rapid tool wear. This poses problems in grinding of magnesium alloy
composites.

Before conducting the experiments for studying the grindability aspects of

magnesium alloy (AZ91D) composites with metal bonded diamond wheel, preliminary
experiments have been conducted with SiC wheel to understand about the response of
magnesium alloy composite. Grinding of magnesium alloy reinforced with SiC, using SiC
wheel usually results in clogging of magnesium at wheel and attrition wear of SiC abrasive
of the wheel. Hence it was decided to use super abrasive wheel. Unlike the investigations
into the machining of traditional metallic materials, relatively little study has been carried out
on grinding of metal matrix composite materials.

Very limited literature is available on grinding of Aluminium reinforced with SiC

particles. Almost, no literature is available on grinding of magnesium alloy composites.
Magnesium is highly oxidizable, fine magnesium powder and chips created in machining
operations can cause fire. There is a risk of burning of chips or powders, if ignited. The
machining process of the components must be performed under controlled conditions, with
extinguishing agents ready on the spot.

vi

Fully replicated 3 factor and 3 level (33) full factorial designed experiments were
conducted for thorough investigation of the process parameters. For all experimental runs,
three replicates were carried out and the average value of each set of data was taken.
Grinding of magnesium composite was carried out by varying process parameters such as
wheel peripheral speed, workpiece velocity and depth of cut. During the process the forces
were monitored by a piezoelectric dynamometer.

The performance of the grinding was studied by analyzing and comparing the
grinding forces, specific grinding energy, and the average surface roughness. The ground
surface was analyzed using optical and scanning electron microscopy. The grinding forces
were observed to be decreasing with the increase in hardness which in turn resulted in
smooth surfaces. The obtained surface roughness (Ra) values were in the range of 0.6- 1.3
m. The surface integrity of the ground surface was analyzed using focused ion beam
machine. There were almost no surface damages on the ground surface. Altered sub surface
layer could be observed in the case of lower volume reinforced composite.

Optimal grinding conditions are to be determined for economic grinding of metal

matrix composites. Despite extensive research on grinding process, determining the desirable
operating conditions in industrial setting still relies on the skill of the operators and trial and
error methods. In the present work, an attempt has been made to optimize the grinding
conditions. Multi objective function model, with surface roughness and tangential force as
user definable constraints was used. Mathematical models were developed using the
experimental data considering only the significant parameters. Optimization was carried out

vii

to obtain the parameters for minimum surface roughness and minimum force using GA. The
results were validated using confirmation tests.

Keywords: Magnesium alloy composite, two step stir casting, grinding, surface integrity.

viii

TABLE OF CONTENTS

Title
Abstract
Acknowledgement
List of figures
List of tables
Notation

Page
No
i
iii
xiv
xviii
xxi

CHAPTER 1
1

INTRODUCTION
1.1

Background

1.2

Metal matrix composites

1.3

Magnesium and magnesium alloy

1.3.1

Effect of alloying elements

11

1.3.2

Classification of magnesium alloy

12

1.4

1.5

1.6

Cast alloy development

14

1.4.1

Magnesium-Aluminum alloy

14

1.4.2

Magnesium-Zirconium alloy

15

Reinforcement

16

1.5.1

Silicon Carbide (SiC)

18

1.5.2

Yttrium Oxide (Y2O3)

19

Applications of magnesium, magnesium alloy and magnesium

19

composites
1.7

1.8

Processing techniques for magnesium based composites

24

1.7.1

Powder metallurgy

24

1.7.2

Squeeze casting

25

1.7.3

Infiltration process

25

1.7.4

Spray deposition

26

1.7.5

Stir casting

26

1.7.6

Two step stir casting

29

Flammability of magnesium

29
ix

1.9

Heat treatment

30

1.9.1

31

Heat treatment of composites

1.10 Characterization of composites

32

1.11 Grinding

33

1.11.1 Abrasives

34

1.11.2 Grinding parameters

36

1.11.3 Surface integrity

37

1.11.4 Surface roughness

40

1.12 Importance of optimization

40

1.13 Summary

41

1.14 Organization of thesis

43
CHAPTER 2

LITERATURE SURVEY
2.1

Introduction

45

2.2

Importance of magnesium, magnesium alloy and its composites

45

2.3

Manufacturing processes for magnesium matrix composites

48

2.3.1

Stir casting

50

2.3.2

Powder metallurgy

59

2.3.3

Squeeze casting

60

2.4

Grindability studies on magnesium and magnesium alloy composites

61

2.5

Optimization

64

2.6

Summary

67

2.7

Motivation

68

2.8

Objectives

69
CHAPTER 3

FABRICATION AND CHARACTERIZATION OF MAGNESIUM

ALLOY BASED COMPOSITES
3.1

Introduction

71

3.2

Materials

71

3.2.1

72

3.3

Preparation of magnesium alloy (AZ91D)

Fabrication of magnesium alloy composites

x

73

3.3.1

Rule of mixture

73

3.3.2

Processing stages of two step stir casting

73

3.3.3

Casting procedure

75

3.3.4

Heat treatment

76

3.4

Porosity measurement

77

3.5

Microstructure characterization

78

3.6

Elemental analysis

79

3.7

X-Ray diffraction studies

79

3.8

Mechanical properties

79

3.8.1

Hardness

79

3.8.2

Tensile testing

80

3.8.3

Fracture behavior

81

3.9

Results and discussion

82

3.9.1

Micro structure

82

3.9.2

X-Ray diffraction studies

84

3.9.3

Elemental analysis

87

3.9.4

Porosity

89

3.10 Mechanical properties

90

3.10.1 Hardness

92

3.10.2 Yield strength

94

3.10.3 Tensile properties

97

3.10.4 Youngs modulus

98

3.10.5 Ductility

100

3.10.6 Fracture behavior

101

3.11 Conclusion of magnesium alloy reinforced with silicon carbide

103

(AZ91D/SiCp)
3.12 Magnesium alloy reinforced with yttrium oxide

104

3.12.1 Density

104

3.12.2 Micro hardness

104

3.12.3 Microstructural studies

106

3.12.4 Elemental analysis

107
xi

3.12.5 X-ray diffraction studies

109

3.12.6 Mechanical properties

110

3.12.7 Fractography

112

3.13 Conclusion of magnesium alloy reinforced with yttrium oxide

115

(AZ91D/Y2O3)
3.14 Summary

116
CHAPTER 4

GRINDING OF MAGNESIUM ALLOY COMPOSITES

4.1

Introduction

119

4.2

Design of experiments

119

4.3

Experimental setup

121

4.4

Selection of workpiece material

122

4.5

Selection of process parameters

122

4.6

Selection of wheel

124

4.6.1

Type of abrasive

124

4.6.2

Type of bond

125

4.6.3

Grit size

125

4.6.4

Grit density

125

4.6.5

Specification of diamond grinding wheel

126

4.7

Specification of grinding machine

127

4.8

Surface roughness measurement

128

4.9

Force measurement

129

4.9.1

130

Charge amplifier

4.10 Dynoware

131

4.11 Surface and subsurface damage analysis

131

4.12 Experimental result and analysis

133

4.12.1 Grinding force

135

4.12.1 (a) Normal grinding force

135

4.12.1 (b) Tangential grinding force

135

4.12.2 Specific grinding energy

136

4.13 Analysis of variance (ANOVA)

141
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4.14 Surface roughness

151

4.15 SEM analysis

155

4.16 FIB milling

159

4.17 Summary

162
CHAPTER 5

MULTI OBJECTIVE OPTIMIZATION

5.1

Introduction

165

5.2

Mathematical formulation

165

5.2.1

Regression analysis

167

5.2.2

Model for tangential force

169

5.2.3

Model for surface roughness

171

5.3

Genetic algorithm (GA)

173

5.3.1

GA Vs traditional methods

175

5.3.2

Working principle of GA

175

5.4

Multi objective optimization using genetic algorithm

180

5.5

Attributes of GA

182

5.6

Results and discussion

184

5.7

Confirmation tests

189

5.8

Summary

190
CHAPTER 6

CONCLUSION AND FUTURE SCOPE

6.1

Conclusion

191

6.2

Future Scope

196

References

197

List of publications from this research work

213

Bio-Data

214

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