Combustion synthesis: Self-propagating high-temperature synthesis (SHS) and decomposition combustion synthesis (DCS) for production of calcium phosphate biomaterials

iii LIST OF FIGURES . viii LIST OF TABLES . xi ACKNOWLEDGEMENTS . xii CHAPTER 1 PROJECT MOTIVATION AND INTRODUCTION . 1 1.1 Bone Replacement Materials . 1 1.2 Shortcomings of Current Calcium Phosphate Production Processes. 2 CHAPTER 2 LITERATURE REVIEW . 4 2.1 Combustion Synthesis Fundamentals . 4 2.2 Calcium Phosphate Fundamentals . 8 2.2.1 Hydroxyapatite (HA) . 8 2.2.2 Tricalcium Phosphate (TCP) . 11 2.2.3 Multiphasic Calcium Phosphates . 13 2.3 Bone Anatomy and Physiology Fundamentals . 14 2.3.1 Structure of Bone . 14 2.3.2 Cortical and Cancellous Bone . 14 2.3.3 Mechanical Properties of Bone . 15 2.3.4 Bone Remodeling Cycle. 16 2.4 Design Requirements for a Bone Substitute Material . 17 CHAPTER 3 EXPERIMENTAL MATERIALS AND METHODS . 19 3.1 Self-Propagating High-Temperature Synthesis of Calcium Phosphate Experimental Procedure (Appendices A and B) . 19 v 3.1.1 HSC Chemistry Analysis . 22 3.2 Post-Synthesis Characterization . 22 3.2.1 Scanning Electron Microscopy and Electron Dispersive Spectroscopy. 23 3.2.2 Brunauer–Emmett–Teller Surface Area Analysis and Barrett–Joyner–Halenda Pore Size and Pore Volume Analysis . 23 3.2.3 X-ray Diffraction (Appendix E) . 23 3.3 Post-Synthesis Collagen, Alginate and Chitosan Coatings . 24 3.3.1 Type I Collagen Coating . 24 3.3.2 Immunofluorescence Labeling (Appendix F) . 24 3.3.3 Alginate Coating . 25 3.3.4 Chitosan Coating . 25 3.3.5 Fourier Transform Infrared Spectroscopy . 25 3.4 Post-Synthesis Characterization-Mechanical Testing . 26 3.5 Antimicrobial Activity Experimental Procedure . 26 3.5. 1 Inductively Coupled Plasma-Atomic Emission Spectroscopy . 26 3.5. 2 Contact Angle Measurements (Appendix G) . 27 3.6 Human Fetal Osteoblast 1.19 Cell Line Cell Culture Procedure (Appendix H) . 27 3.6. 1 Cell Culture Experimental Procedure . 27 3.6. 2 Cell Culture Scanning Electron Microscopy . 28 3.6. 3 Cell Culture Field Emission-Scanning Electron Microscopy . 28 3.7 Statistical Analysis . 28 4.1 Self-Propagating High-Temperature Synthesis Reaction Characterization . 29 4.1.1 Reactant Data . 31 4.1.2 Self-Propagating High-Temperature Synthesis Reaction Data . 31 4.2 Post-Synthesis Characterization-Product Morphology and Composition . 37 4.2.1 Scanning Electron Microscopy of Calcium Phosphate Particles and Sections . 37 vi 4.2.2 Product Microporosity Analysis From Scanning Electron Microscopy Micrographs . 42 4.2.4 X-ray Diffraction of Calcium Phosphate Particles . 47 4.2. 5 Crystal Size and Lattice Strain Analysis from X-ray Diffraction Data . 52 4.3 Post-Synthesis Collagen, Alginate and Chitosan Coatings . 55 4.3.1 Type I Collagen Attachment . 55 4.3.2 Chitosan and Alginate Coatings . 56 4.3.3 Fourier Transform Infrared Spectroscopy of Coated Constructs . 57 4.4 Post-Synthesis Characterization-Mechanical Properties . 59 4.5 Post-Synthesis CharacterizationAntimicrobial Activity and Biocompatibility of Calcium Phosphate Constructs Substituted with Silver . 63 4.5. 1 Antimicrobial Activity of Calcium Phosphate Construct Substituted with Silver . 63 4.5. 2 Inductively Coupled Plasma-Atomic Emission Spectroscopy of Silver Substituted Calcium Phosphate Constructs . 65 4.5. 3 Biocompatibility of Silver Substituted Calcium Phosphate Powders . 65 4.5. 4 Contact Angle Measurements . 66 4.6 Summary of Experimental Results . 68 CHAPTER 5 BIOLOGIC POTENTIAL OF CALCIUM PHOSPHATE BIOPOWDERS PRODUCED VIA DECOMPOSITION COMBUSTION SYNTHESIS FOR BONE TISSUE ENGINEERING . 69 5.