• Bulletin of the Korean Chemical Society
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• v.28 no.10
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• pp.1661-1664
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• 2007

Direct reaction of elemental silicon with a gaseous mixture of isopropyl chloride (1) and hydrogen chloride in the presence of copper catalyst using a stirred bed reactor equipped with a spiral band agitator gave isopropyldichlorosilane having a Si-H bond (2a) as a major product and isopropyltrichlorosilane (2b) along with chlorosilanes, trichlorosilane and tetrachlorosilane. A process for production of 2a was maximized using the 1:0.5 mole ratio of 1 to HCl and smaller size of elemental silicon at a reaction temperature of 220 °C. When a reaction was carried out by feeding a gaseous mixture of 1 [12.9 g/h (0.164 mol/h)] and HCl [2.98 g/h (0.082 mol/h)] to a contact mixture of elemental silicon (360 g) and copper (40 g) under the optimum condition for 45 h, 2a among volatile products kept up about 82 mol % until 35 h and then slowly decreased down 68 mol % in 45 h reaction. Finally 2a was obtained in 38% isolated yield (based on 1 used) with an 85% consumption of elemental silicon in a 45 h reaction. In addition to 2a, 2b was obtained as minor product along with chlorosilanes, trichlorosilane, and tetrachlorosilane. The decomposition of 1 was suppressed and the production of 2a improved by adding HCl to 1.

• Korean Chemical Engineering Research
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• v.49 no.5
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• pp.577-581
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• 2011

Silicon nanoparticles have attracted a great deal of scientific interests due to its intense photoluminescence in the visible spectral region and its potential applications in biological fluorescence maker, RGB (red, green, blue) display, photonics and photovoltaics etc. Practical applications making use of optical and physicochemical properties of Si nanoparticles requires an efficient synthetic method which allows easy modulation of their size, size distribution as well as surface functionalities etc. In this study, a one-pot solution reduction scheme is attempted to prepare alkyl-terminated Si nanoparticles (<10 nm) with Si precursors, (Octyl)$SiCl_3$ or mixture of (Octyl)$SiCl_3$ and $SiCl_4$, containing alkyl-groups using Na(naphthalide) as reducing agent. The surface capping of Si nanoparticles with octyl-groups as well as Si nanoparticle formation was achieved in one-pot reaction. The hexane soluble Si nanoparticles with octyl-termination were in the range of 2-10 nm by TEM and some oxide groups (Si-O-Si) was present on the surface by EDS/FTIR analyses. The optical properties of Si nanoparticles measured by UV-vis and PL evidenced that photoluminescent Si nanoparticles with alkyl-termination was successfully synthesized by solution reduction of alkyl-containing Si precursors in one-pot reaction.