SCI和EI收录∣中国化工学会会刊

中国化学工程学报 ›› 2020, Vol. 28 ›› Issue (9): 2248-2255.DOI: 10.1016/j.cjche.2020.06.023

• Separation Science and Engineering • 上一篇    下一篇

Integrated UV-based photo microreactor-distillation technology toward process intensification of continuous ultra-high-purity electronic-grade silicon tetrachloride manufacture

Ye Wan1,2,3,4, Wenhui Guo5, Jin Xiao1,4, Dazhou Yan2,3, Xiong Zhao2,3, Shuhu Guo2,3, Jianhua Liu2,3, Qifan Zhong1,4, Tao Yang2,3, Yu Zhao3, Xin Chang3, Xin Gao3,5   

  1. 1 School of Metallurgy and Environment, Central South University, Changsha 410083, China;
    2 China ENFI Engineering Co., Ltd., Beijing 100038, China;
    3 National Engineering Laboratory of Polysilicon Materials Preparation Technology, Luoyang 471023, China;
    4 National Engineering Laboratory of Efficient Utilization of Refractory Nonferrous Metal Resources, Central South University, Changsha 410083, China;
    5 School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
  • 收稿日期:2020-03-26 修回日期:2020-06-14 出版日期:2020-09-28 发布日期:2020-10-21
  • 通讯作者: Ye Wan, Xin Gao
  • 基金资助:
    The authors appreciate the financial support from Industry Base Project supported by Ministry of Industry and Information Technology (0714-EMTC02-5593/13) and Scientific Research and Development of Henan province (174200510014).

Integrated UV-based photo microreactor-distillation technology toward process intensification of continuous ultra-high-purity electronic-grade silicon tetrachloride manufacture

Ye Wan1,2,3,4, Wenhui Guo5, Jin Xiao1,4, Dazhou Yan2,3, Xiong Zhao2,3, Shuhu Guo2,3, Jianhua Liu2,3, Qifan Zhong1,4, Tao Yang2,3, Yu Zhao3, Xin Chang3, Xin Gao3,5   

  1. 1 School of Metallurgy and Environment, Central South University, Changsha 410083, China;
    2 China ENFI Engineering Co., Ltd., Beijing 100038, China;
    3 National Engineering Laboratory of Polysilicon Materials Preparation Technology, Luoyang 471023, China;
    4 National Engineering Laboratory of Efficient Utilization of Refractory Nonferrous Metal Resources, Central South University, Changsha 410083, China;
    5 School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
  • Received:2020-03-26 Revised:2020-06-14 Online:2020-09-28 Published:2020-10-21
  • Contact: Ye Wan, Xin Gao
  • Supported by:
    The authors appreciate the financial support from Industry Base Project supported by Ministry of Industry and Information Technology (0714-EMTC02-5593/13) and Scientific Research and Development of Henan province (174200510014).

摘要: Ultra-high-purity silicon tetrachloride (SiCl4) is demanded as an electronic-grade chemical to meet the stringent requirements of the rapidly developing semiconductor industry. The high requirement for ultra-high-purity SiCl4 has created the need for a high-efficient process for reducing energy consumption as well as satisfying product quality. In this paper, a mass of production technology of ultra-high-purity SiCl4 was successfully developed through chlorination reaction in the ultraviolet (UV)-based photo microreactor coupled with the distillation process. The influences of key operational parameters, including temperature, pressure, UV wavelength and light intensity on the product quality, especially for hydrogen-containing impurities, were quantified by the infrared transmittance of Fourier transform infrared spectroscopy (FT-IR) at 2185 cm-1 and 2160 cm-1 indicating that characteristic vibrational modes of Si—H bonds, as well as the operating conditions of distillation were also investigated as key factors for metal impurities removing. The advanced intensification of SiCl4 manufactured by the integration of photo microreactor and distillation achieves the products with superior specifications higher than the standard commercial products.

关键词: SiCl4, Process intensification, Photochlorination, Microreactor, Distillation

Abstract: Ultra-high-purity silicon tetrachloride (SiCl4) is demanded as an electronic-grade chemical to meet the stringent requirements of the rapidly developing semiconductor industry. The high requirement for ultra-high-purity SiCl4 has created the need for a high-efficient process for reducing energy consumption as well as satisfying product quality. In this paper, a mass of production technology of ultra-high-purity SiCl4 was successfully developed through chlorination reaction in the ultraviolet (UV)-based photo microreactor coupled with the distillation process. The influences of key operational parameters, including temperature, pressure, UV wavelength and light intensity on the product quality, especially for hydrogen-containing impurities, were quantified by the infrared transmittance of Fourier transform infrared spectroscopy (FT-IR) at 2185 cm-1 and 2160 cm-1 indicating that characteristic vibrational modes of Si—H bonds, as well as the operating conditions of distillation were also investigated as key factors for metal impurities removing. The advanced intensification of SiCl4 manufactured by the integration of photo microreactor and distillation achieves the products with superior specifications higher than the standard commercial products.

Key words: SiCl4, Process intensification, Photochlorination, Microreactor, Distillation