Si nanoparticles are new prospective optoelectronic materials. Unlike bulk Si cry-stals, Si nanoparticles display intriguing room-temperature photoluminescence. A major challenge in the fabrication of Si nanoparticles is the control of their size distribution. The rare-earth element Er has unique photo emission properties, including low pumping power, and a temperature independent, sharp spectrum. The emission wavelength matches the transmission window of optical fibers used in the telecommunications industry. Therefore, the study of Er-doped Si nanoparticles may have practical significance. The goals of the research described in this dissertation are to investigate vapor phase pyrolysis methods and to characterize the microstructure and associated defects, particles size distributions and photoluminescence efficiencies of doped and undoped Si nanoparticles using analytical transmission electron microscopy, high resolution electron microscopy, and optical spectroscopy. Er-doped and undoped Si nanoparticles were synthesized via vapor-phase pyrolysis of disilane at Texas Christian University. To achieve monodisperse size distributions, a process with fast nucleation and slow growth was employed. Disilane was diluted to 0.48% with helium. A horizontal pyrolysis oven was maintained at a temperature of 1000 °C. The oven length was varied from 1.5 cm to 6.0 cm to investigate the influence of oven length on the properties of the nanoparticles. The Si nanoparticles were collected in ethylene-glycol. The doped and undoped Si nanoparticles have a Si diamond cubic crystal structure. Neither Er precipitation, Er oxides or Er silicides were detected in any of the samples. The Er dopant concentration was about 2 atom% for doped samples from the 3.0 and 6.0 cm ovens as determined by quantitative analysis using X-ray energy dispersive spectroscopy. The average Si nanoparticle size increases from 11.3 to 15.2 nm in the doped samples and from 11.1 to 15.7 nm in the undoped samples as the oven length increases from 1.5 to 6.0 cm. HREM data show that average Si nanocrystallite size varies from 6.4 to 3.3 to 5.9 nm in the doped samples, and from 7.5 to 12.2 nm in the undoped samples as the oven length increases. Room-temperature Er photoluminescence has been detected near 1.54 :m from all doped samples. Saturation of the Er photoluminescence intensity at large emission power and the monotonic decrease of the intensity as a function of the emission wavelength in the doped sample from the 3.0 cm oven suggest that a carrier-mediated energy transfer process occurs in the Er-doped Si nanoparticles. It is the first time to successfully fabricate and investigate Er-doped Si nanoparticles.