“Germanium and supplements” JSC, Novomoskovsk, Tula Region, Russia

V. M. Ivanov, Foreman, e-mail: v.m.ivanov@rambler.ru

The process of hydrogenation of silicon tetrachloride in the polycrystalline silicon production is actual still. The method of catalytic hydrogenation of silicon tetrachloride to trichlorosilane is perspective for use in the industrial production of polysilicon. Previous work on various aspects of the problem is presented. Performed works was carried out in boundaries of laboratory research. The task was set to develop an industrial converter for this process. The granulometric composition of ground silicon, which is used in the hydrogenation process, is presented. The equations of chemical reactions occurring during the process are given. The hydrogenation process is carried out at a temperature of 600 oC and a pressure of 1.1 MPa. Based on the criterion equations, the calculation of the kinetic characteristics of the fluidized bed of ground silicon was performed. The operating speed of the gas-vapor mixture in the reaction part of the converter is determined to be 0.12 m/s. The obtained characteristics were used in calculating the design parameters of the converter for a production capacity of 1000 tons of polysilicon per year. The reaction zone of an industrial converter has an inner diameter of 1.5 m and a height of 10 m. A schematic picture of the converter is shown. The design features of the converter with a cylindrical side-bar are described. The separator is designed for settling particles carried away from the suspended layer. In the gas distributor, the circular arrangement of holes promotes the formation of a fluidized bed. In the converter design, it is advisable to provide louver baffles that improve the characteristics of the fluidized bed. Incoloy 800HT was proposed as a constructive material. The calculation and the proposed design of the converter can be used in the design of equipment for the construction and modernization of polycrystalline silicon production.

1. Kritskaya T. V., Shvartsman L. Ya. New industrial technology for producing polycrystalline silicon “Silicon from sand”. Abstracts of reports of the XII International Conference “Silicon-2018”. Chernogolovka, 2018. p. 8.
2. Ivanov V. M. Chlorination in molten salt in the technology of polycrystalline silicon production. Elektronika NTB. 2019. No. 6. pp. 154–160. DOI: 10.22184/1992-4178.2019.187.6.154.160
3. Ivanov V. M., Trubitsin Yu. V. Application of methods for silicon tetrachloride hydrogenation in polysilicon production technology. Materialy elektronnoy tekhniki. 2010. No. 4. pp. 10–13.
4. Lehnen R. J. Untersuchengen zur katalysierten hydrochlorierung vom metallurgischen silizium mit siliziumtetrachlorid und wasserstoff in einem laborfestbettreaktor: dis. … zur erlangung des grades Dr. rer. nat. Ruhr-Universität Bochum, 2002. 159 s.
5. Ivanov V. M., Trubitsyn Yu. V. Exploratory laboratory studies of catalysts for silicon tetrachloride hydrogenation. Collection of abstracts of the Ukrainian scientific conference on semiconductor physics “UNKFN-5”. Uzhgorod, October 9–15, 2011 Uzhgorod, 2011. p. 419.
6. Becker F. Modellierungen und simulationen der hydrochlorierung von silizium zu trichlorsilan fur die entwicklung eines technischen wirbelschichtreaktors: dis. … zur Erlangung des Grades Dr.-Ing. Rheinisch-Westfälischen Technischen Hochschule, 2005. 143 s.
7. Arkadyev A. A. Development of methods for trichlorosilane synthesis at elevated pressure: Dissertation of Candidate of Engineering Sciences. Moscow, 2005. 139 p.
8. Vorotyntsev A. V. Catalytic reduction of silicon chlorides: Dissertation of Candidate of Chemical Sciences, N. Novgorod, 2013. 121 p.
9. Arkadyev A. A., Kokh A. A., Chapygin A. M., Novikov A. V., Shvarev K. P. Definition of specific speed of low-temperature heterogeneous hydrogenation of silicon tetrachloride. Tsvetnye Metally. 2010. No. 9. pp. 56–58.
10. Fluidized bed reactors: principles and applications. Kristian Beike editor. NY : Nova Science Publication, Inc., 2020. 117 p.
11. Falkevich E. S., Pulner E. O., Chervonny I. F. et al. Semiconductor silicon technology. Moscow : Metallurgiya, 1992. 407 p.
12. Zverev S. V., Nagorny S. L., Trubitsyn Yu. V. Technological aspects of implementation of the high-temperature silicon tetrachloride hydrogenation process. Slozhnye sistemy i protsessy. 2003. No. 1. pp. 81–91.
13. Pavlov K. F., Romankov P. G., Noskov A. A. Examples and tasks for the course on processes and apparatus of chemical technology. Leningrad: Khimiya, 1987. 575 p.
14. Shanlin Du, Guoqiang Lv, Wenhui Ma, Guangkai Gu, Boqiang Fu. Optimal design of gas distributor in fluidized bed for synthesis of silicone monomer. Particuology. 2023. Vol. 83. pp. 115–128. DOI: 10.1016/j.partic.2023.02.015
15. Ning Liu, Xingping Liu, Fumin Wang et al. CFD simulation study of the effect of baffles on the fluidized bed for hydrogenation of silicon tetrachloride. Chinese Journal of Chemical Engineering. 2022. Vol. 45. pp. 219–228. DOI: 10.1016/j.cjche.2021.04.003