Processing of functional inorganic materials including zero (0-D) dimensional (e.g. nanoparticles), 1-D (nanorods, nanofibers), and 2-D (films/coating) structures is of fundamental and technological interest. This research will have two major sections. The first part of section one focuses on the deposition of silicon dioxide onto a pre-deposited molybdenum disilicide coating on molybdenum substrates for both high (>1000 °C) and moderate (500-600 °C) temperature oxidation protection. Chemical vapor deposition (CVD/MOCVD) techniques will be utilized to deposit the metal suicide and oxide coatings. The focus of this study will be to establish optimum deposition conditions and evaluate the metal oxide coating as oxidation - thermal barriers for Mo substrates under both isothermal (static) and cyclic oxidation conditions.;The second part of this section will involve a systematic evaluation of a boron nitride (BN) interface coating prepared by chemical vapor deposition. Ceramic matrix composites (CMCs) are prospective candidates for high (>1000 °C) temperature applications and fiber- matrix interfaces are the dominant design parameters in ceramic matrix composites (CMCs). An important goal of the study is to determine a set of process parameters, which would define a boron nitride (BN) interface coating by a chemical vapor deposition (CVD) process with respect to coating.;In the first part of the second section, we will investigate a new approach to synthesize ultrafine metal oxides that combines microwave heating and an in-situ ultrasonic mixing of two or more liquid precursors with a tubular flow reactor. Different metal oxides such as nickel ferrite and zinc aluminate spinels will be studied. The synthesis of metal oxides were investigated in order to study the effects of the nozzle and microwave (INM process) on the purity, composition, and particle size of the resulting powders.;The second part of this research section involves a study of microwave frequency effects on the synthesis of nanocrystalline tetragonal barium titanate. The effects of microwave frequency (fixed and variable), microwave bandwidths sweep time, and aging time on the microstructure, particle sizes, phase purity, surface areas, and porosities of the as-prepared BaTiO3 were systematically investigated.;The final part of the research involves a new rapid and facile synthetic route to prepare size-tunable, ultranarrow, high surface area OMS-2 nanomaterials via open-vessel microwave-assisted refluxing preparations without employing templates or surfactants. The particle size control is achieved by varying the concentration or type of non-aqueous co-solvent. The structural, textural, and catalytic application properties of the prepared nanomaterials are investigated.