Efficient use of petroleum, coal and natural gas resources requires the use of novel materials and developing technologies. Aerogel-supported nanoparticles are materials with great potential in development of new technologies in energy generation, fuel processing, and by-product remediation. Aerogels represent one of the highest surface area materials known, providing an excellent support for catalytic reactions, including those important in the reformation of petroleum resources. The properties and capabilities of these materials may be modified by tuning the porosity, controlling the size and nature of nanoparticles on the support, and varying the reaction conditions. Our focus in this work is the development of oxygen carriers (aerogel with metal nanoparticles) for application in a Chemical Looping Combustion (CLC) system, a process by which the energy is generated from fuel oxidation where the fuel and oxidant are not in direct contact. The structure and composition of the produced materials in our lab was characterized by X-ray Diffraction, Scanning Election Microscopy, Transmission Electron Microscopy, BET, X-ray Photoelectron Spectroscopy, and Inductively Coupled Plasma Mass Spectrometry. Thermogravimetric Analysis was then employed to optimize the reaction conditions and determine which materials presented the greatest potential for CLC. iii ACKNOWLEDGEMENT I would like to express my sincere appreciation to my research advisor Dr. R. Lloyd Carroll, for his patience, guidance and great support for my research and graduate studies. He provided me with opportunities to learn many new techniques along with a plethora of new experiences. I would additionally like to thank the other members of my committee, Dr. Dady Dadyburjor and Dr. Charter D. Stinespring for their excellent instruction and enlightening discussions. I would also like to thank all the professors and staff involved with WV-Nano, who patiently and kindly trained me on their instruments and techniques. Especially I would like to thank Dr. Andy Woodworth, Dr. Kolin Brown, Eric Shires, Dr. Vin Berry, Dr. M. S. Seehra, they helped me a lot on my research.