Deposition of functional biomedical coating via drop on demand micro dispensing technique

DEPOSITION OF FUNCTIONAL BIOMEDICAL COATING VIA DROP-ON-DEMAND MICRO-DISPENSING TECHNIQUE CHANG LEI National University of Singapore 2013 DEPOSITION OF FUNCTIONAL BIOMEDICAL COATING VIA DROP-ON-DEMAND MICRO-DISPENSING TECHNIQUE CHANG LEI (B.Eng., Northeastern University, China) A THESIS SUBMITTED FOR THE DEGREE OF DOCTOR OF PHILOSOPHY DEPARTMENT OF MECHANICAL ENGINEERING NATIONAL UNIVERSITY OF SINGAPORE 2013 Declaration Declaration I hereby declare that the thesis is my original work and it has been written by me in its entirety I have duly acknowledged all the sources of information which have been used in the thesis This thesis has not been submitted for any degree in any university previously Chang Lei 30 September 2013 i Abstract Abstract Silicon-substituted hydroxyapatite (SiHA) and silver-substituted hydroxyapatite (AgHA) have been shown to provide enhanced bioactivity and anti-bacterial properties over pure hydroxyapatite (HA), respectively In this work, a dual-layer nanoSiHA-nanoAgHA/nanoHA (nSiHA-nAgHA/nHA) coating consisted of a bottom nHA layer and a top hybrid nSiHA-nAgHA layer was developed and fabricated via the Drop-on-Demand (DoD) micro-dispensing technique, to achieve fast bone growth and reduce bacterial adhesion Phase-pure nHA, nSiHA containing 0.7 wt.% silicon (Si), and nAgHA containing 0.5 wt.% silver (Ag) powders were synthesised in-house via a wet precipitation method, and deposited onto the glass substrates using the DoD technique Dispensing parameters were optimised using Taguchi method with an L16 orthogonal array The S/N ratio and ANOVA analysis revealed that the parameters of on-time and pressure had more significant effects on the droplet formation The dual-layer coating retained its physicochemical properties of as-synthesised powders, and exhibited a thickness of 34.5 ± 1.0 µm It exhibited a critical load of 69 mN before failure, and Si and Ag were uniformly distributed on the top layer In addition, adipose-derived stem cells grew and differentiated well on the dual-layer coatings, with up-regulated expression of alkaline phosphatase activity, type I collagen and osteocalcin The growth of S.aureus was inhibited on the dual-layer coating within 24 h In short, this report evaluates the capability of DoD micro-dispensing technique for the deposition of dual-layer nSiHA-nAgHA/nHA coatings, and explores the ii Abstract physicochemical, mechanical and biological properties of coatings, indicating its potential usage in the orthopaedic implants iii Acknowledgements Acknowledgements First of all, I would like to express my deepest appreciation to my supervisors, Prof Thian Eng San and Prof Jerry Fuh Ying Hsi, for their valuable guidance, scientific advices and the best encouragement throughout the entire duration of my research This Ph.D degree and dissertation would not have been possible to be completed without their great support It was my fortune to have this precious opportunity to study with these two greatest supervisors Special thanks go to Prof Wong Yoke San and Prof Hong Geok Soon for their valuable comments in project related issues I would like to thank Dr Sun Jie for her continuous support, scientific suggestions and encouragement on my research I would like to express my special thanks to Ms Lim Poon Nian for her greatest help and support She gave me a lot of valuable advices and helped me solved many research-related problems My sincere thanks also go to all the people in BioFab and Biomat Lab: Ms Li Jinlan, Ms Guo Yilin, Ms Chen Juexuan, Mr Wu Yang, Mr Jie Zequn, Ms Zhang Qinyuan, Ms Lam Ruey Na, Ms Tan Yi Min, Mr Wang Zuyong and Mr Feng Yong Yao Jason for their kindest help and enthusiastic encouragement throughout my Ph.D study My sincere gratitude goes to Ms Lee Lan Yin, Mr Li Jinfu, Dr Yang Rui, Dr Zhang Ming, Dr Li Erqiang, Dr Zhou Jinxin, Mr Ng Jinh Hao, Dr Wang Yan, Ms Xu Qian, Ms Wu Yaqun, iv Acknowledgements Mr Lim Jing, Mr Thian Chen Hai Stanley and Dr Ma Sha for their assistance and knowledge in carrying out the project They are also my friends and make my graduate study in Singapore colourful and memorable My sincere gratitude also goes to the exceptional staffs of Advanced Manufacturing Lab (AML), Material Science Lab and Tissue-Inspired Engineering Lab (NTU) for their support and technical expertise in overcoming many difficulties encountered during the research Last but not least, I dedicate this small achievement to my family for their love, understanding, patience and inspiration v Publications Publications Journal Articles L Chang, J Sun, J.Y.H Fuh, E.S Thian Deposition and characterization of a dual-layer silicon- and silver- containing hydroxyapatite coating via a dropon-demand technique RSC Advances, (28) (2013) 11162-11168 L Chang, E.S Thian, J Sun, J.Y.H Fuh, G.S Hong, Y.S Wong, W Wang Fabrication of functionally-graded hydroxyapatite/titanium oxide coating via drop-on-demand technique NanoLIFE, (1) (2012) 12500091-12500098 E.S Thian, L Chang, P.N Lim, B Gurucharan, J Sun, J.Y.H Fuh, B Ho, B.Y Tay, E.Y Teo, W Wang Chemically-modified calcium phosphate coatings via drop-on-demand micro-dispensing technique Surface & Coatings Technology, 231 (2013) 29-33 J Sun, L Chang, E.S Thian, J.L Li, J.Y.H Fuh, G.S Hong, Y.S Wong, E.J.W Wang Bio-inspired organic-inorganic composite coatings for implants via a micro-dispensing technique Advanced Materials Research, 500 (2012) 662-672 vi Publications Conference Proceedings  L Chang, E.S Thian, J Sun, J.Y.H Fuh Synthesis and characterization of functionally-graded nano-hydroxyapatite/titania bioactive coating via dropon-demand technique Proceedings of the International Symposium on Nanoscience and Technology, (2011) 14-17 Conference Presentations (Oral Presentation) J Sun, L Chang, E.S Thian, J.L Li, J.Y.H Fuh, G.S Hong, Y.S Wong, E.J.W Wang Bio-inspired organic-inorganic composite coatings for implants via a micro-dispensing technique 10th Asia-Pacific Conference on Materials Processing, Jinan, China, 14th June – 17th June 2012 L Chang, E.S Thian, J Sun, J.Y.H Fuh Synthesis and characterization of functionally-graded nano-hydroxyapatite/titania bioactive coating via dropon-demand technique International Symposium on Nanoscience and Technology, Tainan, Taiwan, 18th November – 19th November 2011 E.S Thian, L Chang, B Gurucharan, J Sun, J.Y.H Fuh, W Wang Chemically-modified calcium phosphate coatings via drop-on-demand inkjet printing Taiwan Association for Coating and Thin Films Technology Conference, Kenting, Taiwan, 20th November – 23rd November 2011 vii Publications L Chang, E.S Thian, J Sun, J.Y.H Fuh, W Wang Micro-dispensing of nano-hydroxyapatite (nHA) thin coating on biomedical implants 6th International Conference on Materials for Advanced Technologies, Singapore, 26th June - 1st July 2011 Conference Presentations (Poster Presentation) L Chang, J Lee, S Maleksaeedi, B.Y Tay, E.S Thian Dip-coated nanohydroxyapatite films on metallic 3D 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International Symposium on Nanoscience and Technology, (2011) 14-17 Conference... 2.4.3 Ion Beam Assisted Deposition 57 2.4.4 Sol-Gel Deposition 58 2.4.5 Comparison of Current Coating Techniques for Calcium Phosphate Coatings 59 2.4.6 Proposed Drop- on- Demand