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Novel electrodeposition strategies have been developed for the fabrication of thick adherent zirconia ceramic and composite coatings for biomedical applications. The new method is based on the electrophoretic deposition (EPD) of polyelectrolyte additives combined with the cathodic precipitation of zirconia. The method enables the room- temperature electrosynthesis of crystalline zirconia nanoparticles in the polymer matrix. Adherent crack-free coatings up to several microns thick were obtained. The deposits were studied by thermogravimetric and differential thermal analysis, X-ray diffraction analysis, scanning and transmission electron microscopy, and atomic force microscopy. Obtained results pave the way for electrodeposition of other ceramic-polymer composites. Novel advanced nanocomposite coatings based on bioceramic hydroxyapatite (HA) have been developed for the surface modification of orthopaedic and dental implant metals. HA nanoparticles prepared by a chemical precipitation method were used for the fabrication of novel HA-chitosan nanocomposite coatings. The use of chitosan enables room-temperature fabrication of the composite coatings. The problems related to the sintering of HA can be avoided. A new electrodeposition strategy, based on the EPD of HA nanoparticles and electrochemical deposition of chitosan macromolecules, has been developed. The method enabled the formation of dense, adherent and uniform coatings of various thicknesses in the range of up to 60μm. Bioactive composite coatings containing 40.9-89.8 wt% HA were obtained. The deposit composition and microstructure can be tailored by varying the chitosan and HA concentrations in the deposition bath. A mathematical model describing the formation of the HA-chitosan composite deposit has been developed. X-ray studies revealed preferred orientation of HA nanoparticles in the nanocomposites. Obtained coatings provide corrosion protection of the substrates and can be utilized for the fabrication of advanced biomedical implants. For further functionalization of the HA-chitosan composite coating, Ag and CaSi03 have been incorporated into the coating. Novel HA-Ag-chitosan and HA-CaSiO3-chitosan nanocomposite coatings have been deposited as monolayers, laminates, and coatings of graded composition. The obtained results can be used for the development of biocompatible antimicrobial coatings with controlled Ag+ release rate, and nanocomposite coatings with enhanced bioactivity. / Thesis / Doctor of Philosophy (PhD)

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京都大学 / 新制・課程博士 / 博士(工学) / 甲第23913号 / 工博第5000号 / 新制||工||1780(附属図書館) / 京都大学大学院工学研究科物質エネルギー化学専攻 / (主査)教授 作花 哲夫, 教授 安部 武志, 教授 阿部 竜 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DGAM

<p> Pure zinc and zinc/yttria stabilized zirconia (YSZ) composite coatings for combined wear and corrosion protection of ferrous substrates were prepared by electrodeposition using acidic zinc sulphate solutions containing YSZ and gelatin. The morphology of the electrodeposit was studied by Field Emission Scanning Electron Microscopy (FESEM) with energy dispersive spectroscopy (EDS). X-ray diffraction was employed to determine the texture of the zinc deposits. In the electrodeposition of pure zinc coatings, the influence of electrodeposition parameters, including current density, deposition time and solution pH was studied. It was found that the deposition rate was controlled by the current density and that an increase in deposition time resulted in the formation of deposit microstructures with coarse, columnar grains. The deposits prepared from solutions with lower pH were composed of uniform, fine grains and exhibited a basal plane preferred orientation.</p> <p> The effects of gelatin on zinc electrodeposition were investigated. It was found that the addition of gelatin profoundly modified the microstructure and crystallographic orientation of the zinc deposit. As the gelatin concentration increased, the mean grain size of zinc deposit was reduced and the basal plane preferred orientation was inhibited. The modification of the microstructure and orientation by gelatin increased microhardness of the zinc coating. However, the corrosion protection property which was assessed by potentiodynamic polarization test was not significantly changed.</p> <p> In the study on composite coatings, the incorporation of ceramic particles in the zinc deposit was characterized as a function of the deposition solution composition. The effect of ceramic particles on the hardness of the composite coatings was assessed by microhardness. The corrosion potential of the composite coating was determined by potentiodynamic polarization tests. The results showed that decrease in solution pH and addition of gelatin promoted the co-deposition of ceramic particles with zinc. The mechanical and corrosion properties of conventional zinc coatings were improved by the incorporation of ceramic particles.</p> / Thesis / Master of Applied Science (MASc)