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Faculty of Manufacturing Engineering FABRICATION AND CHARACTERISTIC STUDY OF ALUMINA TOOL USING COLD ISOSTATIC PRESS Abdul Aziz Bin Adam Master of Manufacturing Engineering (Industrial Engineering) 2014 © Universiti Teknikal Malaysia Melaka

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Faculty of Manufacturing Engineering

FABRICATION AND CHARACTERISTIC STUDY OF ALUMINA

TOOL USING COLD ISOSTATIC PRESS

Abdul Aziz Bin Adam

Master of Manufacturing Engineering (Industrial Engineering)

2014

© Universiti Teknikal Malaysia Melaka

FABRICATION AND CHARACTERISTIC STUDY OF ALUMINA

TOOL USING COLD ISOSTATIC PRESS

ABDUL AZIZ BIN ADAM

A thesis submitted in fulfillment of the requirements for the degree of Master of Manufacturing

Engineering in Industrial Engineering

Faculty of Manufacturing Engineering

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

2014

© Universiti Teknikal Malaysia Melaka

DECLARATION

I declare that this thesis entitled "Fabrication and Characteristic Study of alumina Tool

Using Cold Isostatic Press" is the result of my own research except as cited in the

references. The thesis has not been accept for any degree and is not concurrently submitted

in candidature of any other degree.

Signature

Name

Date

Abdul Aziz Bin Adam

25th August 2014

© Universiti Teknikal Malaysia Melaka

APPROVAL

I hereby declare that I have read this report and in my opinion this thesis is sufficient in

terms of scope and quality for the award of Master of Manufacturing Engineering

(Industrial Engineering).

Signature

Supervisior Name

Date

. ............ ... r. ...... ..... ........ . Dr. Mohd Sanusi Bin Abdul Aziz

<f'/9 / lol't

DR. MOHD SANUSI llN AIDUl AZIZ Swtior Lectww

Faculty of Manufacturin9 Engineering Universitf Teknlli•I •lcsyli• M.iali•

Hant Tueh Jay• 76100 Durian r.,,....,, MAia•

© Universiti Teknikal Malaysia Melaka

DEDICATION

This thesis is dedicated to my beloved mother, father, siblings and friends. They have been

a source of motivation and strength during moments of despair and discouragement,

support has been shown in incredible ways recently.

© Universiti Teknikal Malaysia Melaka

ABSTRACT

In manufacturing, machining is widely used in the production. The selection of a suitable tool will boost production performance and reduce costs. In this study, alumina cutting tools are fabricated and its characteristics information gained through various experiments. Numbers of previous studies using alumina -based composite cutting tool were done and mostly agreed that the alumina based have the potential to produce a homogeneous ceramic cutting inserts with high performance. However, less research were found for the production of alumina milling cutting insert . Therefore, this study focuses on the application of cold isostatic press to produce alumina cutting insert that has a good microstructure and mechanical properties. The characteristic of cutting insert that has been produced then tested through various experiments and test. The inserts produce accordance to triangle shaped inserts. Alumina powder with purity of 91.4 % was used to produce the cutting tool. The powder then compressed through cold isostatic pressure techniques. The pressure applied is range of 15,000 psi, 20,000psi and 25 ,000 psi. Green body and then dried and sintered at two different temperatures of and 1400 °C and 1550 °C. The density, hardness and shrinkage of alumina milling insert then were studied. Matrix design method was utilized to build experimental and accurate data. Product which were pressed at 20,000 psi and sintered at 1550 °C shows assured result and shall be tested to identify the cutting performance of the inserts.

© Universiti Teknikal Malaysia Melaka

ABSTRAK

Dalam industri pembuatan, pemesinan digunakan secara meluas dalam pengeluaran produk. Pemilihan mata a/at yang sesuai akan membantu memoptimasikan prestasi pengeluaran serta mengurangkan kos. Dalam kajian ini, perkakas pemotong alumina difabrikasi dan sifat-sifat pemotong alumina diuji melalui ujikaji bagi mendapatkan maklumat prestasi sifat perkakas. Beberapa kajian terdahulu menggunakan komposit berasaskan alumina mendapati bahawa perkakas pemotong tersebut berpotensi menghasilkan komponen seramik yang homogen serta berprestasi tinggi. Namun, kurang kajian bagi penghasilan perkakas pemotong kisar alumina. Oleh itu, kajian ini lebih tertumpu kepada aplikasi tekanan sejuk bagi menghasilkan perkakas pemotong alumina yang mempunyai mikrostruktur dan sifat mekanik yang baik. Perkakas yang dihasilkan kemudiannya diuji melalui pelbagai ujikaji bagi mendapatkan maklumat karakter struktur dan mekanikal perkakas. Fabrikasi pembuatan akan mengikut standard komersial TKPN berbentuk segitiga. Fabrikasi perkakas pemotong bermula dengan mendapatkan serbuk alumina ketulenan 91.4%. lni diikuti dengan pembentukanjasad anum perkakas pemotong alumina melalui teknik tekanan sejuk. Tekanan yang dikenakan adalah pelbagai iaitu 15, 000 psi, 20, OOOpsi dan 25, 000 psi. Seterusnya, sampel disinter pada dua suhu yang berbeza iaitu 1400 °C dan 1550 °C. Jasad kemudian dikaji ketumpatan, kekerasan-vikers dan pengecutan Kaedah rekabentuk matrik telah digunakan sepenuhnya untuk membina ujikaji serta data-data yang tepat. Produk yang ditekan di 20, 000 psi dan disinter pada 1550 ° C menunjukkan hasil terjamin dan wajar diuji untuk mengenal pasti prestasi pemotongan serta kualiti pemotongan menggunakan .

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ACKNOWLEDGEMENT

Alhamdulillah, all praises to Allah for the strengths and His blessing in completing this report. I would like to take this opportunity to express my sincere acknowledgement to my supervisor, Dr Mohd Sanusi Bin Abd Aziz from the Faculty of Manufacturing Engineering Universiti Teknikal Malaysia Melaka (UTeM) for his essential supervision and constant support and encouragement toward completion of this report. Not forget special thanks to Dr Raja Izamshah Bin Raja Abdullah for his invaluable help of constructive comments and suggestions. I would also like to express greatest gratitude to Majlis Amanah Rakyat (MARA) for the opportunity and support that been given. Special thanks my beloved parents; siblings and peers for their moral support in completing this report. Lastly, thank you to everyone that have been to crucial participate directly and indirectly in realization this project.

l1l

© Universiti Teknikal Malaysia Melaka

TABLE OF CONTENT

ABSTRACT ABSTRAK ACKNOWLEDGEMENT TABLE OF CONTENT LIST OF TABLES LIST OF FIGURES LIST OF APPENDICES

CHAPTER 1. INTRODUCTION

1.0 Background Study 1.1 Statement of Purpose 1.2 Problem Statement 1.3 Objectives 1.4 Scope

2. LITERATURE REVIEW 2.0 Introduction

2.1 Ceramic Material 2.1.1 Properties of Ceramic 2.1.2 Properties of Alumina

2.2 Cold Isostatic Press 2.2.1 Types of Cold Isostatic Press 2.2.2 Cold Isostatic Processing 2.2.3 The Pressure Chamber

2.3 Rubber Mould 2.4 CIP Process on Alumina Oxide (Ah03) Powder 2.5 Sintering 2.6 High Speed Milling 2.7 Ceramic Milling Inserts 2.8 Silicon Nitride as Cutting Tool Material 2.9 Previous Study

3. RESEARCH METHODOLOGY 3.0 Introduction 3.1 Project Methodology 3.2 Experimental Matrix 3.3 Sample Preparation

3.3.1 Alumina Powder 3.3.2 Dry Pre-Press By Uniaxial Press Machine 3.3.3 Cold Isostatic Press 3.3.4 Furnace 3.3.5 X-Ray Fluorescence

IV

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PAGE

11

iii iv VI

vii x

1 2 2 3 3

4 6 6 7 9 10 11 12

14 15 16 18 19 22 24

26 28 28 30 32 32 34 35 38

4.

5.

6.

3.4 Responce Measurement 3.4. l Hardness Measurement 3.4.2 Density Measurement and Water Absorption 3.4.3 Linear Shrinkage 3.4.4 Thermal Expansion 3.4.5 Flexural Test I Modulus of Rupture 3.4.6 Fracture I Charpy Impact Test

RESULT 4. l Introduction 4.2 The Element Composition Analysis 4.3 Green Density (Before Sintering) 4.4 Density After Sintering 4.5 Water Absorption 4.6 Shrinkage (Green Compact) 4. 7 Shrinkage After Sintered 4.8 Thermal Expansion 4.9 Hardness 4.10 Flexural Strength (Modulus of Rapture) and Flexural Modulus

4.10.1 Flexural Strength 4.10.2 Flexural Modulus

4.11 Impact Test

DISCUSSION 5.1 Mechanical analysis

5.1.1 Green Density 5.1.2 Sintered Density 5.1.3 Water Absorption 5.1.5 Shrinkage 5. l . 6 Hardness 5.1. 7 Flexural Strength

CONCLUSIONS AND RECOMMENDATIONS 6.1 Conclusion

REFERENCES

APPENDICES

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38 38 39 41 41 43 44

46 47 49 50 55 59 60 63 64 68 68 69 69

71 71 72 72 73 74 75

76

78

82

TABLE

2.1

2.2

2.3

2.4

2.5

2.6

2.7

3.1

3.2

3.3

3.4

3.5

3.6

4.1

LIST OF TABLES

TITLE

Properties of various ceramic at room temperature

General properties of alumina powder

Properties of polyurethane

Operating pressure guidelines for various powder

Common inserts shape codes

Typical inserts tolerances

Common inserts hole configuration

Selected process parameters and number of levels

Pressing pressure 15 Kpsi with sintering temperature

Pressing pressure 20 Kpsi with sintering temperature

Pressing pressure 25 Kpsi with sintering temperature

Detailed specification of cold isostatic press machine

Firing Program

Analyse Concentration Table of Alumina TM-DAR using XRF

PAGE

7

9

15

16

21

22

22

29

29

29

30

34

37

48

4.2 The comparison between experimental and theoretical alumina density 53

4.3 Percentage water absorption of alumina powder sintered at l 400°C 56

4.4 Percentage water absorption of alumina powder sintered at 1550°C 57

4.5 Outcomes of impact test 70

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LIST OF FIGURES

FIGURE TITLE PAGE

2.1 Arrangements of ions of 0 2· A13

+ inside Ah03 8

2.2 Micrograph of alumina powder 8

2.3(a) Schemetic diagram of dry bag CIP 10

2.3(b) Schemetic diagram of wet bag CIP 10

2.4 Process of wet bag cold isostatic pressing 11

2.5 Process of wet bag dry isostatic pressing 12

2.6 Full threaded cover 13

2.7 Breech lock pressure chamber type 13

2.8 Pin Closure ASME type 14

2.9 Rubber mould sample 15

2.10 Sintering mechanisme on particle densification 17

2.11 Types of milling process 19

2.12 Standard nomenclature mill cutting inserts configuration 20

3.1 Process Flow 27

3.2 Double sided triangular insert 32

3.3 (a) DORST uniaxial machine 33

3.3 (b) Triangular inserts 33

3.3 (c) Pre-press alumina inserts 33

3.4 Wet bag isostatic press machine 35

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© Universiti Teknikal Malaysia Melaka

3.5

3.6

3.7

3.8

3.9

3.10

3. 11

4.1

4.2

4.3

4.4

4.5

4.6

4.7

4.8

4 .9

N abertherm furnace l 600°C

Firing profile for 1400 °C

Firing profile for 1550 °C

ESEway Digital Vickers Hardness Testers

Dilatometer

Universal Tensile Machine - GOTECH 50 KN

GOTECH Impact Tester

Alumina tringular shaped milling inserts

Density of green product before sintered at 1400°C

Density of green product before sintered at 1550°C

Density of alumina sintered at l 400°C at different pressure

Density of alumina sintered at l 400°C at different pressure

Densification of alumina sintered at temperature l 400°C

Densification of alumina sintered at temperature l 550°C

Percentage of water absorption at sintered temperature of 1400°C

Percentage of water absorption at sintered temperature of l 550°C

36

36

37

39

42

43

45

47

49

50

51

52

53

53

58

58

4.10 Percentage shrinkage alumina powder after CIP press at 15,000 psi 60

4.11 Percentage shrinkage alumina powder after CIP press at 20,000 psi 60

4.12 Percentage shrinkage alumina powder after CIP press at 25,000 psi 60

4.13 Shrinkage percentages versus various pressing pressure and sintering

4.14

4.15

temperature

Shrinkage trends

Thermal expansion data of Alumina TM-DAR

62

62

64

4.16 Vickers hardness value respect to varies pressing pressure and sintered at

temperature l 400°C 65

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4.17 Vickers hardness value respect to varies pressing pressure and sintered at

temperature I 550°C

4.18 Hardness trends respect to pressing pressure and sintering

temperature

66

67

4.19 Flexural strength of alumina TM-DAR respect to pressing pressure and

sintering temperature

4.20 Variation of flexural modulus with pressing pressure and sintering

temperature

4.21 Variation in impact energy respect to pressing pressure and sintering

temperature

ix

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68

69

70

APPENDIX No.

A

B

LIST OF APPENDICES

TITLE

Results of Experiments (Raw data)

Standard Test Method

x

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CHAPTER 1

INTRODUCTION

1.0 Background Study

Isostatic presses are widely used to produce pre-form of high density and

dimensionally precise products. Isostatic presses shall satisfy fabrication of one elongated

dimension products, a complex shape even large volume products (J.S. Reed 1995). One of

product that can be produce by isostatic presses is cutting tools. In the manufacturing

industry, machining is widely used in the production of products. A tool is considered

reliable when it can machined the workpiece with relative ease while producing the desired

range of surface finish. The characteristics of a tool with good machineability are when

less power needed to cut, can cut in a short time, produced good surface finish and less

wear in a short period of usage.

Selection of appropriate cutting tools is very important to produce products with

high dimensional accuracy and surface finish quality. Properties of alumina (Ah03) which

is high hardess, wear resistance and chemical stability makes it become highly suitable as a

research topic to develop its capability as cheap and reliable cutting tool. Ceramic tools

materials with alumina based facing increasing interest as they exhibit high hardness,

thermal resistance and high abrasion resistance, thus making it suitable for high speed

machining (K. Geric 2010).

This project were designed to understand the effect of CIP process on physical

behavior of alumina oxide (Ah03) powder to produce a milling cutting insert with respect

to shrinkage, hardness and densification.

© Universiti Teknikal Malaysia Melaka

1.1 Statement of the Purpose

Machining technology facing increasing interest since it improve productivity and

produce better workpiece surface quality. Continual improvements consistantly done either

by increasing the wear resistant or improving the material used to produce the cutting tools.

Development of advanced ceramic tools increasingly active in past decades which ceramic

material can significantly increase the tool life relative to ceramic special qualities. Most of

the research focus on alumina coated with other materials. Basically, less research were

done on fabricating alumina inserts which will be used in milling.

1.2 Problem Statement

Cold isostatic press (CIP) is one of the pressing techniques that available to

manufacture cerannc inserts. Developing ceramic insert through powder technology

involve with various parameters such as pressing pressure, pressing time and grain size of

the alumina powder. These parameters significantly affect the mechanical and physical

properties of compacted product before and after sintering process such as density,

hardness, strength and dimensional accuracy.

High-speed machining technology has already penetrated in most manufacturing

industries to cut various workpiece from steel and alloys to composites. Manufacturing

engineers frequently use high-speed milling to remove the greatest possible quantity of

material from workpiece. However, using high-speed milling leads to the increase of

cutting temperature and soften of the tool material (Liu et al 2002). Therefore, tool material

with high wear resistance take a crucial role in high-speed milling.

Demand on high performance cutting tool lead to production of cutting tool with

low cost. Alternative material shall be studies to replace conventional material used to

produce cutting tool such as carbides, high speed steels and tungsten. Research that has

been done on alumina tool in high speed machining area is mostly on turning machines.

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Unfortunately, studies on alumina cutting inserts for milling process still not many.

Traditional ceramic fabrication used alumina matrix with additives then pressed using hot

pressed. The weakness by using this technique, compromising on the hardness and wear

tool are inevitable. Pressing using cold isostaic gives promising idea on producing alumina

cutting inserts.

1.3 Objectives

The main objectives of this research as follows:

i. To study the effect of CIP parameters on shrinkage, hardness and densification

behaviour of alumina oxide after undergo Cold Isostatic Press process.

11. To develop ceramic cutting insert of alumina oxide (Ah03) using Cold Isostatic

Press.

1.4 Scope

In this research, the scope of this project are outline as follows:

l. Prepress sample using uniaxial press machine, Cold Isostatic Press (CIP) process

and sintering process will be employed in producing the ceramic cutting tool.

2. The material used for ceramic cutting tools will Alumina Oxide (Ah03).

3. The input parameters that will be used are cold isostatic pressing pressure and

sintering temperature.

4. The product to be fabricate according to commercial milling insert with triangular

shape.

5. The output responces to be investigated include shrinkage, hardness, prorsity,

densification and flexural strength behavior of alumina cutting insert.

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CHAPTER2

LITERATURE REVIEW

2.0 Introduction

The trend toward high speed machining, dry cutting and the need of complex

geometry tool cause an increasing demand for ceramic based material as cutting tools for

machining steel based alloys in machining industries nowadays. Because of these reasons,

the ceramic materials such as alumina and zirconia which are well known as hard and

brittle materials are being developed as cutting tools to penetrate the tooling market.

Ceramic engineering or advanced ceramics are inorganic non-metallic materials used in

high-performance engineering applications. It can be categorized as oxide-based ceramics,

carbides, nitrides and borides (Xu & Jahanmir 1996). Among the properties of advanced

ceramics are wear and oxidation resistance, high stability against chemical reaction, stable

against thermal resistance, thermal insulation and electrical insulation. Research and

development of ceramic material are very intensive in order to increase its potential as a

high quality cutting tools. The use of ceramics cutting tool has increased due to its ability

to operate at high temperatures and resistant to oxidation and chemical reactions (Lee

1999).

The needs and interest on ceramic mcrease especially in machining field .

Machining is a metal forming process and preferable technique in manufacturing industry

due to its simple operation and relatively fast in certain aspect. High speed machining

operations require cutting tools that are resistant in terms of temperature and pressure.

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Some common cutting tools used in machining operations include high speed steel,

carbide, ceramic, cement, diamond and cubic boron nitride.

Ceramic cutting tools are considered as a suitable alternative of carbide or high

speed steel. It can perform machining operations on both high and low velocity effectively

(Lo Casto et al. 1996). Among the ceramic cutting tools most widely used in the market is

alumina. Alumina ceramics are among the most notable because it has a high hardness and

high stability against temperature and the chemistry (Xu et al. , 2001 ). It is also cheaper

than ceramic nitrides and carbides (Xu & Jaharnnir 1996). Number of studies has been

done in developing the potential of alumina as cutting tools, particularly in terms of the

strength properties. Presently, there are several kinds of alumina-based composite insertion

tool such as alumina-zirconia, alumina-titanium-carbide, alumina-zircon, alumina-silicon-

carbide (K. Geric 2010, Xu et al. 2001 ).

Cold isostatic press (CIP) is one of the pressing or compaction techniques that

available in the manufacturing of ceramic inserts. Compaction process can produce near

net shape, density, and particle-to-particle contact which make the part sufficiently strong

for further processes (S.Kalpakjian 2001 ). CIP have a wide range of applications such, as a

repair work for casting product or fabrication of metal matrix composite (MMC) and

ceramic matrix composite (CMC). Few researches on CIP process on ceramic powder were

done. Most researches that have been done were focus on other processes such as slip

casting and dry pressing (uniaxial).

This project aims to understand the effect of CIP and sintering process such as

temperature and pressure on the physical behaviour of powder ceramic part with respect to

shrinkage, hardness, density, flexural strength, Modulus of rupture and fracture strength.

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2.1 Ceramic Material

Ceramics are inorganic, non-metalic materials which the metallic and non-metalic

elements bonded together primarily by ionic or covalent bonds. Ceramic divided to three

basic categories:

I. Traditional ceramics: Silicates for clay products such as pottery.

2. New ceramics: non-silicates ceramics such as oxides and carbides. These

categories poses better mechanical or physical properties compared to

traditional ceramics.

3. Glass: based primarily on silica and having non-crystalline structure.

New ceramics material relatively has high strength, high temperature resistance,

high wear resistance and good corrosion resistance. New ceramics further classified into

three distinct categories of oxides, non-oxides and composites. Examples of oxides

ceramics are alumina (Ah03) and zirconia (ZrO). Non-oxides materials are carbides,

borides, nitrides and silicide. Meanwhile composites ceramic are reinforced material and

combinations of oxides and non-oxides.

2.1.1 Properties of Ceramic

In general ceramics are hard, brittle, electric and heat resistance, wear resistance

and chemically inert. Physical properties of various ceramics are shown in Table 2.1.

Generally, ceramic have low density compared to metals but higher than polymers. The

melting temperature of ceramics is higher than most metals. In term of electrical and

thermal conductivity, mostly they are insulators but in certain condition they can be good

conductor. For thermal expansion, most ceramic having less thermal expansion compared

to metals but the effect are more damaging due to brittleness properties of ceramic.

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Table 2. l: Properties of various ceramic at room temperature. (S.Kalpakjian 2001)

Comprc i\'C la tic Material ymbol tren2th Modu lus Hardne, Den ity

(Mpa) ( Pa) (HK) (kg/m 1

)

lumina Oxide Al:?O , 1000-2900 JI 0-410 2000-3000 4000-4 00

Cu bi boron nitride C B ' 7000 50 4000- 000 J480

ilicon nitride Si :; 4 No data J00-310 2000-2500 J300

Si licon carbide SiC 700-J500 240-480 2 100-JOOO 3100

Titanium carbide TiC JI 00-3850 J 10-410 1800-3200 5500-5800

Tung ten carbide WC 4100-5900 520-700 1800--400 I 0000- I 5000

2.1.2 Properties of Alumina

Alumina is an oxide ceramic used either in pure form or as a mixture with other

oxides. Alumina occurs naturally in large quantities and is available via the Bayer process

(J.S. Reed 1995). Naturally, the alumina exists in two forms, namely a-Al203 and y-

Al203. a -Al203 is stable elements when compared with y -Al203. Alumina structure

consists of oxygen ions in the close packed hexagonal structure. In Al203, Al3 + ions are

placed in octahedral interstices makes each ion is surrounded by six 02-ions. Figure 2.6

shows the arrangement of ions in the vicinity of the 02-ions Al3 + in Al203 polyhedron

structure (Callister 2001 ). Alumina is very hard crystalline, having hexagonal close pack

array of oxygen atoms with metal atoms in two-thirds of octahedrally cordinates interstites.

Each metal atom cordinated by six oxyen atoms and each having four metal neighbours

(6:4 coordination). Figure 2.1 show the arrangement of oxygen ion and aluminum ions for

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alumina. Chemical formula of alumina is Ah03 shows the it compounds of aluminium and

oxygen. They are available in concentration of99.5% and 96 % purities. The microstucture

of alumina is shown in Figure 2.2. Structure containing alumina powder is known as

mullite and spinel, which usually used as refractory materials for high temperature

applications. Table 2.2 shows the general specifications of high-purity alumina material.

Figure 2.1 Arrangements of ions of 0 2- AI3+ inside Ah03.

(Source: Callister, 2001)

Figure 2.2: Micrograph of alumina powder. (Source: Callister, 2001)

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Table 2.2 : General properties of alumina powder. (Lo Casto et. al 1996)

Aluminium Oxide 99.9% Purity

General

Molecular formula Ah03

Molar mass l 01.96 g/mol

Properties

Density and phase 3.97 g/cm3, solid

Solubality in water Insoluble

Melting point 2054 °C

Boiling point -3000 °C

Thermal conductivity 18 W/m.K

Hardness - V ikers 18 Gpa

Modulus Elasticity 350 GPa

Thermal Expension 8.5 x 1 o-<>;oc

Fracture Toughness, Kie 4.6 Mpa m1' L

2.2 Cold Isostatic Press

CIP is used extensively in powder metallurgy which include ceramics industry.

Isostatic pressing capable to deligate uniform high pressure to produce parts. The product

is consistent in density throughout their cross sections compared to parts that produced by

uniaxial press. CIP comes in two types; dry bag and wet bag. Dry bag process is molding

powder that filled in a forming rubber mold as shown in Figure 2.3(a). Forming process

done by transmitting pressure through a pressing rubber mold in high- pressure vassel. The

limitation of dry bag CIP is limited to small size parts and simple shapes where products

can be removed easily. In the wet bag press, the pressure vassel is filled with liquid,

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