Electrophoretic deposition of multifunctional polymer-bioactive glass composite coatings Elektrophoretische Abscheidung von multifunktionalen Kompositschichten aus Polymer und bioaktivem Glas der Technischen Fakultät der Friedrich-Alexander Universität Erlangen-Nürnberg zur Erlangung des Doktorgrades Dr.-Ing. vorgelegt von Dipl.-Ing. Sigrid Gertraud Seuß aus Erlangen Als Dissertation genehmigt von der technischen Fakultät der Friedrich-Alexander-Universität Erlangen-Nürnberg Tag der mündlichen Prüfung: 29. Januar 2016 Vorsitzende des Promotionsorgans: Prof. Dr. Peter Greil Gutachter/in: Prof. Dr.-Ing. habil. Aldo. R. Boccaccini Prof. Dr. sc. techn. Sannakaisa Virtanen Publications Partial results of this work have been published or presented in presentations or poster presentations in advance. Publication S. Seuss, M. Lehmann, A.R. Boccaccini; Alternating Current Electrophoretic Deposition of Antibacterial Bioactive Glass-Chitosan Composite Coatings. Int. J. Mol. Sci, 15, 12231-12242, 2014. S. Seuss, M. Heinloth, A.R. Boccaccini; Development of bioactive composite coatings based on combination of PEEK, bioactive glass and Ag nanoparticles with antibacterial properties. Surface & Coatings Technology, In Press. Presentations Design of Experiment (DoE) for the electrophoretic deposition of Polyetheretherketone (PEEK) coatings; EPD Conference, October 2011, Puerto Vallarta, Mexico. Electrophoretic Deposition of PEEK-Bioglass® composite coatings; NBBA Seminar, July 2012, Bayreuth. Electrophoretic Deposition (EPD) in Erlangen: Applications of EPD to biomaterials; NBBA Seminar, November 2013, Bayreuth. Poster Electrophoretic deposition of soft polymer‐based composite coatings containing bioactive glass particles; Strategies in Tissue Engineering, 3rd Conference, Wuerzburg, May 2012. Contents Contents Abstract ............................................................................................................................................................. 1 Zusammenfassung........................................................................................................................................... 3 Introduction ...................................................................................................................................................... 5 Chapter 1: Fundamentals .................................................................................................................................... 8 1.1 Introduction ................................................................................................................................................ 9 1.2 Electrophoretic Deposition ..................................................................................................................... 10 1.2.1 DC EPD vs. AC EPD ........................................................................................................................ 12 1.2.2 Suspensions ....................................................................................................................................... 14 1.2.3 Deposition Mechanisms .................................................................................................................. 15 1.2.4 Kinetics ............................................................................................................................................... 17 1.3 Parameter Optimization ......................................................................................................................... 19 Chapter 2: Materials ........................................................................................................................................... 22 2.1 Introduction .............................................................................................................................................. 23 2.2 PEEK .......................................................................................................................................................... 24 2.2.1 Chemical Properties and Processing .............................................................................................. 24 2.2.2 Mechanical Properties ...................................................................................................................... 25 2.2.3 Thermal Properties ........................................................................................................................... 26 2.2.4 Composite Materials ........................................................................................................................ 26 2.2.5 Biocompatibility and Industrial Applications .............................................................................. 27 2.2.6. EPD of PEEK and PEEK Composites ............................................................................................ 27 2.3 Chitosan .................................................................................................................................................... 29 2.3.1 Chemical Properties and Processing .............................................................................................. 29 2.3.2 Biocompatibility and Industrial Applications .............................................................................. 30 2.3.3 EPD of Chitosan and Chitosan Composites.................................................................................. 30 2.4 Bioactive glass .......................................................................................................................................... 32 2.4.1 Chemical Properties and Processing .............................................................................................. 32 2.4.2 Biocompatibility and Industrial Applications .............................................................................. 33 2.4.3 Bioactivity .......................................................................................................................................... 34 2.4.4 Nano-Bioactive Glass ....................................................................................................................... 35 2.4.5 Coatings ............................................................................................................................................. 35 2.5 Antibiotics ................................................................................................................................................. 37 2.6 Silver .......................................................................................................................................................... 39 Chapter 3: Methods ............................................................................................................................................ 42 Contents 3.1 Introduction .............................................................................................................................................. 43 3.2 Electrophoretic Deposition ..................................................................................................................... 44 3.3 Adhesion Tests ......................................................................................................................................... 45 3.4 FTIR ........................................................................................................................................................... 47 3.5 Roughness Measurements ...................................................................................................................... 48 3.6 Contact Angle ........................................................................................................................................... 49 3.7 Thermal Analysis ..................................................................................................................................... 50 3.8 Tests in Simulated Body Fluid ............................................................................................................... 51 3.9 Bacteria Studies ........................................................................................................................................ 53 3.10 Cell Culture Studies ............................................................................................................................... 55 Chapter 4: Electrophoretic Deposition of PEEK/Bioactive Glass Composite Coatings with Antibacterial Properties………………………………………………………………………………………………………...57 4.1 Introduction .............................................................................................................................................. 58 4.2 Electrophoretic Deposition of PEEK ..................................................................................................... 59 4.2.1 Design of Experiment (DoE) ........................................................................................................... 59 4.2.2 Heat Treatment ................................................................................................................................. 67 4.2.3 Crystallinity ....................................................................................................................................... 68 4.2.4 Adhesion Tests .................................................................................................................................. 69 4.2.5 Contact Angle Measurements ........................................................................................................