This thesis mainly consists of two parts, the synthesis of several kinds of technologically interesting crystalline metal oxide nanoparticles via high temperature nonaqueous solution processes and the formation of core-shell structure metal oxide composites using some of these nanoparticles as the core with silica, titania or polymer as shell via a modified microemulsion approach. In the first part, the experimental procedures and characterization results of successful synthesis of crystalline iron oxide (Fe3O4) and indium oxide (In2O3) nanoparticles are reported. Those nanoparticles exhibit monodispersed particle size, high crystallinity and high dispersibility in non-polar solvents. The particle size can be tuned by the seed medi...