| This dissertation reports investigations on the synthesis of metal chalcogenide semiconductor nanoparticles grown within the pores of a nanoporous aluminum oxide template. The template used to restrict the growth of the materials contained cylindrical pores, yielding nanoparticles with non-spherical shapes. Two classes of metal chalcogenides were studied: those with three dimensional structures and those with layered structures.; Three different methods were developed and investigated for the growth of MQ compounds (M = Cd, Zn, Cu, Hg; Q = S, Te): (1) a dipping method, (2) a U-tube method, and (3) a sublimation. The dipping method produced material on the template's outer surface and within the pores only within {dollar}sim{dollar}2 {dollar}mu{dollar}m of their ends. Within the limits of the template pore size, particle size and shape could not be controlled. The U-tube method deposited multiple oval shaped particles within each pore of the template. The oval particles were polycrystalline, had sizes ranging from {dollar}sim{dollar}5-120 nm, and were concentrated in only one location in the pores. Reasons for the uneven distribution of particles throughout the pores were investigated. The sublimation method only deposited material on the outer surfaces of the template, and the conditions used for the sublimation altered the morphology of the template.; Layered MS{dollar}sb2{dollar} compounds (M = Mo, W, Re, Ti) were prepared by the thermal decomposition of selected precursor molecules within the pores of the template. The fibers produced had the same dimensions as the pores of the template. When MoS{dollar}sb2{dollar} was prepared by this method, tubules of oriented crystals were formed with multiple plugs in each tubule. When WS{dollar}sb2{dollar} was prepared, more solid fibers were formed. The preparation of ReS{dollar}sb2{dollar} and TiS{dollar}sb2{dollar} resulted in fibers that were similar in morphology to the MoS{dollar}sb2{dollar} fibers. The effect of template loading method, precursor concentration, precursor type, solvent, presence of a surfactant, and annealing temperature on morphology and crystallinity of MoS{dollar}sb2{dollar} fibers were investigated. Reaction products were characterized compositionally, morphologically, structurally, and optically using SEM, TEM, EDS, electron diffraction, X-ray diffraction, and UV-visible absorption spectroscopy. |