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UNIVERSITI TEKNOLOGI MARA POWDER INJECTION MOULDING OF SYNTHESIZED HYDROXYAPATITE POWDER FROM CLAMSHELL

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UNIVERSITI TEKNOLOGI MARA

POWDER INJECTION MOULDING OF SYNTHESIZED HYDROXYAPATITE

POWDER FROM CLAMSHELL

NURUL HUDA BINTI M. ALI

Thesis submitted in fulfillment of the requirements for the degree of

Master of Science

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AUTHOR'S DECLARATION

I declare that the work in this thesis was carried out in accordance with the regulations of Universiti Teknologi MARA. It is original and is the results of my own work, unless otherwise indicated or acknowledged as referenced work. This thesis has not been submitted to any other academic institution or non-academic institution for any degree or qualification.

I, hereby, acknowledge that I have been supplied with the Academic Rules and Regulations for Post Graduates, Universiti Teknologi MARA, regulating the conduct of my study and research.

Name of Student Student I.D. No.

Programme Faculty Thesis Title

Signature of Student Date

Nurul Huda Binti M. Ali 2012986249

Master of Science (Chemical Engineering) - EH750 Chemical Engineering

Powder Injection Moulding of Synthesized Hydroxyapatite Powder from Clamshell

C ^ y ^ ^ /

August 2015

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ABSTRACT

Hydroxyapatite (HAp) is one of the most versatile bioceramic materials since it is widely used in biomedical and dentistry applications. This research focused on the effect of pH and calcination temperature on synthesized HAp powder from clamshells via chemical precipitation method. Besides that, the process of PIM using synthesized HAp powder mixed with PS based binder system had studied. The effect of sintering temperatures on the as-sintered HAp specimens had evaluated for its physical and mechanical properties.

The process to synthesize HAp powder involves calcination of clamshells powder followed by the titration method using low concentration of phosphoric acid. Based on the analysis, synthesized HAp powder at the temperature of 850°C with the final pH solution of 6.5 has similar characterizations with commercial HAp powder. Then, the process is followed by a green processing route via PIM technique to produce the as- sintered HAp specimen. From the results attained, it shows that synthesized HAp feedstock prepared with the powder loading of 60 vol.% shows pseudo-plastic behavior.

The feedstock was successfully injection moulded according to ASTM standard CI 424- 10 to produce green specimens at the temperature of 200°C with the pressure range from 4 to 7 bars. The green specimens were then successfully debound and sintered through single step wick-debinding and sintering process using alumina powder as an embedment agent. The sintered specimens were than evaluated on physical and mechanical properties. From the results obtained, sintering temperature above 1100°C is not preferable since HAp is start to decompose and forming TCP which not suitable for load bearing applications.

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ACKNOWLEDGEMENT

I would like to express my deep and sincere gratitude to my supervisor, Dr Istikamah Subuki. Her wide knowledge and her logical way of thinking have been of great value for me. Her understanding, encouraging and personal guidance have provided a good basis for the present of the thesis.

I am deeply grateful to my co-supervisor, Dr Muhammad Hussain Ismail and Dr Teng Wang Dung who introduced me to the field of powder injection molding (PIM), whose letters gave me important guidance during my first steps into PIM studies. I would not be performing this work without Dr Hussain's continual encouragement and support. His ideals and concepts have had a remarkable influence on my entire career in the field of PIM research. I also wish to express my warm and sincere thanks for his detailed and constructive comments, and for his important support throughout this work.

I warmly thank to Dr Azuddin Mamat, lecturer in University of Malaya who teach me a lot regarding PIM. Besides that, the opportunity to use injection moulding machine in his workplace had contributed a lot in completing my research study. Without his valuable knowledge and experience, for sure I cannot complete this research study on time.

I would like to extend my gratitude to all lecturers, FKK Postgraduate members and CAMAR of Faculty of Mechanical Engineering,UiTM for discussions, encouragement, support and help in many aspects. I also would like to thank to my beloved family for always keep supporting and advise me throughout for this research work.

Last, and above all, I must give my thanks to God, from whom all blessing flow. It has only been through faith that I have known which direction to travel. May my future endeavors always be a testament to His glory. The financial support from Fundamental Research Grant Scheme (FRGS, 600-RMI/FRGS 5/3 (23/2013) Universiti Teknologi MARA (UiTM) and My Master are gratefully acknowledged.

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TABLE OF CONTENTS

Page

CONFIRMATION BY PANEL OF EXAMINERS ii

AUTHOR'S DECLARATION iii

ABSTRACT iv ACKNOWLEDGEMENT v

TABLE OF CONTENTS vi LIST OF TABLES xi LIST OF FIGURES xiii LIST OF SYMBOLS xvi LIST OF ABBREVIATION xviii

LIST OF CHEMICAL FORMULA xx

CHAPTER ONE: INTRODUCTION 1

1.1 Research Background 1 1.2 Problem Statement 3 1.3 Research Objectives 4 1.4 Scope of the Research 4

1.5 Thesis Outline 6

Referensi

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TABLE OF CONTENTS Page AUTHOR'S DECLARATION i ABSTRACT ii ACKNOWLEDGEMENT iii TABLE OF CONTENTS iv LIST OF TABLES vi LIST OF FIGURES viii LIST OF APPENDIXES ix CHAPTER ONE:

TABLE OF CONTENTS Page STUDENTS'S DECLARATION ii ABSTRACT iii ACKNOWLEDGEMENT iv TABLE OF CONTENTS v LIST OF TABLES viii LIST OF FIGURES ix LIST OF ABBREVIATIONS x CHAPTER

TABLE OF CONTENTS Page AUTHOR’S DECLARATION ii ABSTRACT iii ACKNOWLEDGEMENT iv TABLE OF CONTENTS v LIST OF TABLES vii LIST OF FIGURES viii LIST OF ABBREVIATIONS ii CHAPTER

TABLE OF CONTENTS Page AUTHOR'S DECLARATION ABSTRACT ACKNOWLEDGEMENT TABLE OF CONTENTS LIST OF TABLES LIST OF FIGURES LIST OF PLATES LIST OF ABBREVIATIONS 11 iii iv v

TABLE OF CONTENTS Page TITLE PAGE AUTHOR'S DECLARATION ii ABSTRACT iii ACKNOWLEDGEMENTS iv TABLE OF CONTENTS v LIST OF TABLES xiii LIST OF FIGURES xvi LIST OF PLATES xix LIST

TABLE OF CONTENTS AUTHOR'S DECLARATION ii ABSTRACT iii ACKNOWLEDGEMENT TABLE OF CONTENT LIST OF TABLES vii LIST OF FIGURES LIST OF SYMBOLS ix LIST OF ABBREVIATIONS x CHAPTER

TABLE OF CONTENTS TITLE PAGE AUTHOR'S DECLARATION ACKNOWLEDGEMENT TABLE OF CONTENT LIST OF TABLES LIST OF FIGURES LIST OF PLATES LIST OF ABBREVIATION ABSTRACT CHAPTERl INTRODUCTION

iii TABLE OF CONTENTS TITLE PAGE AUTHOR’S DECLARATION i ACKNOWLEDGEMENT ii TABLE OF CONTENT iii LIST OF TABLES v LIST OF FIGURES vi LIST OF PLATES viii LIST OF