Efficient Preparation of Si3N4 by Microwave Treatment of Solar-Grade Waste Silicon Powder

ACS Omega. 2020 Mar 4;5(11):5834-5843. doi: 10.1021/acsomega.9b04027. eCollection 2020 Mar 24.

Abstract

In this study, the waste silicon powder generated in the production of solar-grade polysilicon scrap was used as the raw material, and silicon nitride (Si3N4) was directly efficient prepared by the microwave heating nitridation. The temperature raising characteristics of silicon powder by microwave heating and the influencing factors of the nitridation reaction process were studied. The thermogravimetric analysis was performed, and the temperature raising dielectric properties of silicon powder were studied. The electromagnetic field and temperature distributions of the microwave heating-induced silicon powder nitridation process were simulated using COMSOL software. The nitridation reaction of silicon powder induced by microwave heating has better temperature raising characteristics: the average heating rate can reach 135 °C/min, and the reaction time is significantly shortened (only 10-20 min). Microwave heating decreases the nitridation reaction temperature by more than 100 °C and greatly shortens the reaction time. With the increase of nitrogen pressure and reaction time, the nitridation reaction is better. In addition, the conversion of the nitridation reaction is more than 97%, and the products are mainly β-Si3N4 with the uniform and columnar morphology. Finally, it is proved that the efficient recovery and utilization of industrial waste silicon powder are realized, and there is lower energy consumption by microwave heating technology.