Direct Electrochemical Preparation of Nanostructured Silicon Carbide and Its Nitridation Behavior

Abstract

Silicon carbide was synthesized from mixtures of SiO2 and graphite by applying the concept of the FFC-Cambridge process and several fundamental aspects of the synthesis route were investigated. Porous disks composed of powders of SiO2 and graphite in molar ratios of 1:0.5, 1:1 and 1:1.5 were prepared by sintering in inert atmosphere and subjected to electro-deoxidation in molten CaCl2 at 1173 K under a range of experimental conditions. Disks of molar ratio 1:1.5, reduced at an applied voltage of 2.8 V for a duration of 6 h, yielded exclusively phase-pure SiC of nanowire morphology as the reaction product, while the other precursor compositions provided significant amounts of calcium silicides. Voltages lower than 2.8 V gave mixtures of SiC with elemental Si and graphite, and voltages higher than that gave CaSi alone. Shorter electro-deoxidation times led to incomplete reduction and allowed for the identification of CaSiO3 as a transient phase. Based on the experimental results a multipath reaction mechanism is proposed, consisting of the electrochemical reduction of SiO2 and CaSiO3 to Si and the subsequent in-situ carbonization of the Si formed to SiC. The effect of N-2 at high temperature on the electrochemically synthesized SiC was investigated and the formation of nanowire Si2N2O was observed. Overall, the process presented is a facile single-step and low-temperature method for the synthesis of SiC with possible commercial prospects. (c) The Author(s) 2018.