Kh. Brookes et al., Effect of Al and Ca addition on the copper catalysed formation of silanes from Si and CH3Cl, APP CATAL A, 206(2), 2001, pp. 257-265
The effect of Al and Ca addition on formation of silanes in the Rochow Dire
ct Process is described and discussed. The catalysts are evaluated in a sti
rred-bed microreactor using on-line gas chromatographic analysis. The forma
tion of silanes from the reaction of Si and CH3Cl is studied using a copper
catalyst in the form of copper chloride. Initial tests using a typical sil
icon source showed that the reactor could be used to follow the consumption
of Si with reproducibility of +/-2%, and similar reproducibility was obser
ved for product selectivity. The reactivity of a pure silicon and an indust
rial silicon sample were compared using the reactor and both samples showed
identical reactivity and selectivity with respect to the amount of silicon
consumed. Addition of Al metal (Cu:AI mole ratio=1.50, 0.30, 0.15) was fou
nd to significantly enhance reactivity and, to a much lesser extent, enhanc
ed selectivity to dichlorodimethylsilane. Addition of CaCl2 (Cu:Ca mole rat
io=0.530, 0.105, 0.053) significantly decreased reactivity but had no marke
d effect on selectivity. Modification of the CuCl catalyst is reported in w
hich CuCl is reacted with silanes and a form of CuCl was synthesised with s
ignificantly increased reactivity but with high selectivity to light produc
ts. (C) 2001 Elsevier Science B.V. All rights reserved.