This dissertation is focused on the development and characterization of a novel class of solid-state nano-structured composites for hydrogen storage based on silica aerogel. It is organized sequentially around experiments conducted to fabricate, optimize and characterize silica aerogel and the composites for hydrogen storage. First, the basics of nano-structured media, silica aerogel technology and solid-state hydrogen storage are introduced. Next, the fabrication and optimization of silica aerogel for hydrogen storage is described in detail. The key result is that varying fabrication parameters can improve the physical properties of the resultant silica aerogel in the context of hydrogen storage. The fabrication of solid-state nano-structured composites using chemical vapor infiltration is then discussed. A series of experiments is used to parameterize the fabrication process, which results in a collection of parameters that minimize variation and structural damage in the composites. Silica aerogel and the composites are then physically characterized using transmission electron microscopy, X-ray diffraction and porosimetry in order to investigate their nano-structuring.

An overview of hydrogen storage characterization and two innovations that improve the accuracy and efficiency of hydrogen storage characterization of low-bulk density media like silica aerogel and the composites are then presented. Finally, the innovations are applied to silica aerogel and the composites to characterize their hydrogen storage performance. Silica aerogel and the composites are found to outperform the most common benchmark in physisorption media, and one composite in particular shows unique hydrogen storage performance.