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

doi:10.1016/j.cjche.2020.06.023

Chinese Journal of Chemical Engineering ›› 2020, Vol. 28 ›› Issue (9): 2248-2255.DOI: 10.1016/j.cjche.2020.06.023

• Separation Science and Engineering • Previous Articles Next Articles

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

Ye Wan^1,2,3,4, Wenhui Guo⁵, Jin Xiao^1,4, Dazhou Yan^2,3, Xiong Zhao^2,3, Shuhu Guo^2,3, Jianhua Liu^2,3, Qifan Zhong^1,4, Tao Yang^2,3, Yu Zhao³, Xin Chang³, Xin Gao^3,5

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:2020-10-21 Published:2020-09-28
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).

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

Ye Wan^1,2,3,4, Wenhui Guo⁵, Jin Xiao^1,4, Dazhou Yan^2,3, Xiong Zhao^2,3, Shuhu Guo^2,3, Jianhua Liu^2,3, Qifan Zhong^1,4, Tao Yang^2,3, Yu Zhao³, Xin Chang³, Xin Gao^3,5

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

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).

Abstract

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

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

Ye Wan, Wenhui Guo, Jin Xiao, Dazhou Yan, Xiong Zhao, Shuhu Guo, Jianhua Liu, Qifan Zhong, Tao Yang, Yu Zhao, Xin Chang, Xin Gao. Integrated UV-based photo microreactor-distillation technology toward process intensification of continuous ultra-high-purity electronic-grade silicon tetrachloride manufacture[J]. Chinese Journal of Chemical Engineering, 2020, 28(9): 2248-2255.

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

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

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