Thesis (M.S., Materials Science) | Growth of metal/oxide nanowires inside of semiconducting nanotubes has several applications for energy storage and energy conversion. In this study, growth of copper/copper oxide through electrodeposition techniques was studied as a method to fill TiO2> nanotube arrays. Specifically, emphasis was placed on the study of copper containing electrolyte solution kinetics. This was necessary due to the differences between TiO2 and anodic aluminum oxide (AAO) as the substrate. AAO has been well-studied and successfully filled with metal/oxide nanowires. The difficulty with TiO2 is that unlike AAO it is not an insulator; this makes electrodeposition of the copper difficult as it is not inherently attracted to the bottom of the nanotubes. Another area of study was the morphology of the TiO2 substrate. Through different anodization techniques a new self-ordered morphology of TiO2 called Super Honeycomb was discovered. Applications of the Super Honeycomb nanostructure as well as a similar process on Ti-Mn alloy are reported.