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Thermoelectric (TE) materials have the capability to convert thermal energy into useful electrical energy. Sustainable energy production and its utilization are among the many challenges that humankind is facing today. In 2016 and 2017, the expected global production of hydrocarbon based automotive vehicles is expected to be 97.8 and 101.8 million respectively, and is expected to rise. The collective thermal energy losses from radiators and exhausts from these automotive vehicles are enormous. This is a big bottleneck in sustainable energy production and utilization. In mitigating this hurdle, TE materials will play a very important role. However, TE materials have low efficiency in thermal to electrical energy conversion owing to the reciprocal relation between the thermal and the electrical transport properties. Recent advances in nanotechnology tools have given a new dimension to decouple this relation. Back in 2003, our group reported a very promising TE material, NiyMo3Sb5.4Te1.6 (y < 0.1). Improving the figure-of-merit of Ni0.05Mo3Sb5.4Te1.6 (“bulk”) material through nanocomposite synthesis is one of the goals of my research. The main outcome of nanocomposite synthesis is the reduced thermal conductivity through arresting the coherent propagation of heat carrying acoustic waves in TE materials. To this end, I synthesized and characterized the transport properties of various nanocomposites. I have used fullerenes, oxides, carbides, and metal particles to fabricate nanocomposites. Chapter 3 addresses the effect of multi-wall carbon nanotubes (MWCNT) when added to Ni0.05Mo3Sb5.4Te1.6. We characterized these samples for …