Energy storage provides sustainability when coupled with renewable but intermittent energy sources such as solar, wave and wind power, and electrochemical supercapacitors represent a new storage technology with high power and energy density. For inclusion in supercapacitors, transition metal oxide and sulfide electrodes such as RuO2, IrO2, TiS2, and MoS2 exhibit rapid faradaic electron–transfer reactions combined with low resistance. The pseudocapacitance of RuO2 is about 720 F/g, and is 100 times greater than double-layer capacitance of activated carbon electrodes. Due to the two-dimensional layered structure of MoS2, it has proven to be an excellent electrode material for electrochemical supercapacitors. Cathodic electrodeposition of MoS2 onto glassy carbon electrodes is obtained from electrolytes containing (NH4)2MoS4 and KCl. Annealing the as-deposited Mo sulfide deposit improves the capacitance by a factor of 40x, with a maximum value of 360 F/g for 50 nm thick MoS2 films. The effects of different annealing conditions were investigated by XRD, AFM and charge storage measurements. The specific capacitance measured by cyclic voltammetry is highest for MoS2 thin films annealed at 500°C for 3h and much lower for films annealed at 700°C for 1 h. Inclusion of copper as a dopant element into electrodeposited MoS2 thin films for reducing iR drop during film charge/discharge is also studied. Thin films of Cu-doped MoS2 are deposited from aqueous electrolytes containing SCN-, which acts as a complexing agent to shift the cathodic Cu deposition potential, which is much more anodic than that of MoS2. Annealed, Cu-doped MoS2 films exhibit enhanced charge storage capability about 5x higher than undoped MoS2 films. Coal combustion is currently the largest single anthropogenic source of CO2 emissions, and due to the growing concerns about climate change, several new technologies have been developed to mitigate the problem, including oxyfuel coal combustion, which makes CO2 sequestration easier. One complication of oxyfuel coal combustion is that corrosion problems can be exacerbated due to flue gas recycling, which is employed to dilute the pure O2 feed and reduce the flame temperature. Refractory metal diffusion coatings of Ti and Zr atop P91 steel were created and tested for their ability to prevent corrosion in an oxidizing atmosphere at elevated temperature. Using pack cementation, diffusion coatings of thickness approximately 12 and 20 µm are obtained for Ti and Zr, respectively. The effects of heating to 950°C for 24 hr in 5% O2 in He are studied in situ by thermogravimetric analyses (TGA), and ex situ by SEM analyses and depth profiling by EDX. For Ti-coated, Zr-coated and uncoated P91 samples, extended heating in an oxidizing environment causes relatively thick oxide growth, but extensive oxygen penetration greater than 2.7 mm below the sample surface, and eventual oxide exfoliation, are observed only for the uncoated P91 sample. For the Ti- and Zr-coated samples, oxygen penetrates approximately 16 and 56 µm, respectively, below the surface. In situ TGA verifies that Ti-and Zr-coated P91 samples undergo far smaller mass changes during corrosion than uncoated samples, reaching close to steady state mass after approximately four hours.

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yes / The tribological performance of a nanocrystalline coating is heavily influenced by its composition, morphology, and microstructural characteristics. This research work describes the effect of heat treatment temperature on the microstructural, morphological, and mechanical behavior of nanocrystalline Ni/TiO2 coatings produced by electrophoresis. The surface morphology and coating cross section were characterized by scanning electron microscopy (SEM). The composition of coatings and the percentage of TiO2 nanoparticles incorporated in the Ni matrix were studied and estimated by using an energy-dispersive spectroscopic (EDS) analysis, while x-ray diffractometry (XRD) was used to investigate the effect of heat treatment temperature on phase structure. The results showed agglomeration of TiO2 nanoparticles on the surface of the coating. The high hardness and wear resistance recorded for the as-deposited coating was attributed to the uniform distribution of TiO2 nanoparticle clusters throughout the cross section of the coating. Heat treatment of the Ni/TiO2 coatings to temperatures above 200 °C led to significant grain growth that changed the surface morphology of the coating and reduced the strengthening effects of the nanoparticles, thus causing a reduction in the hardness and wear resistance of the coatings.

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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