Novel Indirect Additive Manufacturing for Processing Biomaterials Shah Fenner Khan Mohamad Khan This dissertation is submitted for partial fulfilment for the degree of Doctor of Philosophy. School of Mechanical and System Engineering Newcastle University Newcastle upon Tyne, United Kingdom. September 2015 Abstract The aim of this work was to identify methods for the production of patient-specific biomedical devices via indirect additive manufacturing (AM) methods. Additive manufacturing has been shown to provide a good solution for the manufacture of patient specific implants, but in a limited range of materials, and at a relatively high cost. This research project considered what are known as “indirect” AM approaches, which typically consider AM in combination with one or more subsequent processes in order to produce a part, with a maxillofacial plate and mandible resection used as a demonstrator application. Three different approaches were considered: (i) using AM to produce moulds for powder pressing of bioceramic green parts for subsequent sintering; (ii) using AM to produce moulds for biopolymer sintering; and (iii) 3D printing of bioceramic powders into green parts for subsequent sintering. Apatite wollastonite glass ceramic (AW) and poly-Lactide-co-glycolide (PLGA) were selected as the bioceramic and biopolymer materials to process. These were characterised before and after processing in order to ensure that the processing route did not affect the material properties. Geometric dimensions, the morphological structure and mechanical properties were studied to establish the accuracy, shrinkage and strength of the fabricated biomaterial implants. The use of AM processes to produce moulds for PLGA sintering, and the 3D printing of bioceramic powders formed the best overall results in terms of the definition and properties of the manufactured parts. Parts produced were accurate to within 5% of the as designed dimensions for both the PLGA sintering and the bioceramic powders 3D printing. The indirect AM methods are considered to be promising processing routes for medical devices. iii Dedication This work is dedicated to my beloved late parents, Noor Aini Abdullah 1939 – 1984 Mohamad Khan Shoumuz Khan 1937 – 2014 “Semoga Allah swt mencucuri rakhmat ke atas roh mereka. Tiada yang mustahil dicapai sekiranya berusaha tanpa mengalah.” Nothing is impossible to accomplish if one persevere without giving in. iv Personal statement During the time spend in doing this research it had broadened my view as an academician as well as a human being. Doing research is just not about academic materials purely but also involved the interpersonal domain. How one communicates and respects others that surround the daily activities in carrying out the research play an important and significant role in the success of the research. The more one seek to understand one thing the more one will realise the need to understand a lot of others related things. v Declaration This dissertation is the result of my work and includes nothing, which is the outcome of the work done in collaboration except where specifically indicated in the text. It has not been previously submitted, in part or whole, to any university of institution for any degree, diploma, or other qualification. In accordance with the Faculty of Science, Agriculture and Engineering guidelines, this thesis does not exceed 80,000words. Signed: _ _ Date: 23rd September 2015 Shah Fenner Khan Mohamad Khan MSc. (UK), BSc. (USA) Student ID: A079082150 School of Mechanical and Systems Engineering Newcastle University, UK. vi Acknowledgements In the duration of my study in Newcastle University, I am ever grateful to all the individuals who have contributed to my quest of knowledge as a Ph.D. student. First of all, I would to extend gratitude and appreciation to my supervisors Prof. Dr. Kenneth W. Dalgarno and Dr. Matthew German (School of Dental Sciences) for their insightful inputs, invaluable assistance, guidance and supports throughout this research journey. This research would not have been possible without their supervision and encouragement as supervisors and as friends. I too would like to express my appreciation to the technical team; Ken Madden, Malcolm Black, Michael Foster, Stephen Charlton and Brian Stoker for all the technical assistances and helpful advices during practical works. I would also like to thank Andrew Yates (School of Dental Sciences) for assistance in the operation of DSC analysis and Instron tensile testing equipment, Maggie White (School of Chemical Engineering and Advanced Materials) for helping in XRD analysis, Pauline Carrick (ACMA) and Tracey Davey (Medical School) for SEM works and Neville Dickman (School of Chemical Engineering and Advanced Materials) for assistance in operation of Carbolite furnace. My gratitude also extended to Phil Heslop (Computing Science) for 3D printing the parts that were used in the research. I would also like to thanks to my colleagues for their suggestions, wishes and help during the four years study. Furthermore, I would like to thank University Malaysia Perlis and the Malaysian Higher Education Ministry for sponsoring me and giving me the opportunity for doing research in Newcastle University. And most of all, I would like to express my endless love to my family for their understanding and support through the duration of my study. Very special thanks to my children; Nurdiyanah Nasuha, Muhammad Zulhanis, Nurliyanah Atiqah, NurIffah Syahirah and NurIzzah Syakirah, for bringing smiles and laughter. For them, there are my sparks of encouragement to carry on when I am down. Finally, for my ever dearest wife, Salma Mohamad Isa for the wishes, love and support, as well as being always by my side. vii viii Table of Contents Abstract ............................................................................................................................ iii Dedication ........................................................................................................................ iv Personal statement ............................................................................................................ v Declaration....................................................................................................................... vi Acknowledgements ........................................................................................................ vii Table of Contents ............................................................................................................ ix List of Tables .................................................................................................................. xv List of Figures ................................................................................................................ xvi List of Abbreviations and Acronyms ............................................................................ xxi Chapter 1: Introduction ..................................................................................................... 1 1.1 Introduction ............................................................................................................ 1 1.2 Research Problem ................................................................................................... 2 1.3 Research Aim and Objectives................................................................................. 4 1.3.1 Aim .................................................................................................................. 4 1.3.2 Objectives ........................................................................................................ 4 1.4 Research Framework .............................................................................................. 4 1.5 Thesis Outline ......................................................................................................... 5 Chapter 2: Literature Review ........................................................................................... 7 2.1 Introduction ............................................................................................................ 7 2.2 Fundamentals of Additive Manufacturing (AM).................................................... 7 2.3 Process categories of AM Systems ....................................................................... 10 2.3.1 Vat photopolymerisation ............................................................................... 10 2.3.2 Powder bed fusion ......................................................................................... 11 2.3.3 Directed energy deposition ............................................................................ 12 2.3.4 Binder jetting ................................................................................................. 14 2.3.5 Material Jetting .............................................................................................. 15 ix 2.3.6 Material Extrusion.......................................................................................... 15 2.3.7 Sheet Lamination ........................................................................................... 17 2.4 Type of Application in AM ................................................................................... 18 2.4.1 Rapid prototyping .......................................................................................... 20 2.4.2 Rapid tooling .................................................................................................. 20 2.4.3 Rapid manufacturing ...................................................................................... 21 2.5 Indirect AM ........................................................................................................... 22 2.6 Design in AM ........................................................................................................ 23 2.7 STL file format...................................................................................................... 26 2.8 Natural Bone ......................................................................................................... 28 2.8.1 Bone Graft Substitute (BGS) Materials. ........................................................ 29 2.8.2 Fixation of bone graft substitute. ................................................................... 31 2.9 Bioceramic and glass-ceramics ............................................................................. 32 2.9.1 Glass-Ceramic ................................................................................................ 34 2.9.2 Apatite Wollastonite glass-ceramics .............................................................. 37 2.10 Biodegradable polymer ....................................................................................... 39 2.10.1 Polylactide-co-Glycolide Acid (PLGA)....................................................... 43 2.11 Biocomposite ...................................................................................................... 44 2.12 Forming Processes of Biomaterials in the Manufacturing of Medical Devices and Implants ........................................................................................................ 44 2.12.1 Fabrication methods in ceramic material ..................................................... 45 2.12.2 Methods in processing of biopolymers ........................................................ 46 2.13 Sintering .............................................................................................................. 47 2.13.1 Solid-state and liquid state sintering ............................................................ 48 2.14 Materials Characterisations and Analysis ........................................................... 50 2.14.1 Density Measurement using Pycnometer ..................................................... 51 2.14.2 DSC .............................................................................................................. 52 2.14.3 SEM ............................................................................................................. 54 x
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