GB820192A - Process of producing pure silicon - Google Patents

Process of producing pure silicon

Info

Publication number
GB820192A
GB820192A GB22874/57A GB2287457A GB820192A GB 820192 A GB820192 A GB 820192A GB 22874/57 A GB22874/57 A GB 22874/57A GB 2287457 A GB2287457 A GB 2287457A GB 820192 A GB820192 A GB 820192A
Authority
GB
United Kingdom
Prior art keywords
reactor
silane
methane
silicon
carbon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB22874/57A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Allied Corp
Original Assignee
Allied Chemical Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Allied Chemical Corp filed Critical Allied Chemical Corp
Publication of GB820192A publication Critical patent/GB820192A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Pure silicon is produced by the thermal decomposition of silane or partially chlorinated silane in a silica reactor the inside walls of which are lined with a layer of vitreous carbon upon which the silicon is deposited. Methane which may be diluted with an inert gas, e.g. 1-100% methane: 0-99% inert gas preferably 10% methane: 90% inert gas is passed through a silica reactor heated in a furnace to 1000-1200 DEG C. preferably 1000-1100 DEG C. to deposit a vitreous layer of carbon on the inside walls of the reactor. The inert gas may be any noble gas, e.g. helium, neon or argon, or hydrogen, and the reactor may be cylindrical, polygonal or conical in shape. The flow of methane is interrupted and silane vapour or vapour of a partially chlorinated silane, which may be diluted with hydrogen or argon, is passed through the reactor at 600-1200 DEG C. Trichlorosilane is preferably employed at 900-1000 DEG C. When sufficient silicon has collected in the reactor it is allowed to cool to ambient temperature and the product removed. Vitreous carbon contaminating the silicon is removed by mechanical abrasion and/or by immersion in an etching solution of nitric acid (1 part) hydrofluoric acid (2 parts) in water (50%) whereby carbon separates and floats off leaving pure silicon which is washed with aqueous HCl and dried. The reactor after washing and drying is ready for re-use. Pure silane for use in the above process is prepared by reacting purified SiCl4 with LiAlH4 in a continuous manner in excess anhydrous ether over a period of some hours in an atmosphere of H2. Silane so produced is purified by passage together with 2-3 volumes of purified hydrogen through a reflux condenser cooled by dry-ice/acetone, a dry-ice cooled trap, an activated carbon bed, a dry-ice cooled trap and thence to the reactor.ALSO:Pure silicon is produced by the thermal decomposition of silane or partially chlorinated silane in a silica reactor the inside walls of which are lined with a layer of vitreous carbon upon which the silicon is deposited. Methane which may be diluted with an inert gas e.g. 1-100% methane : 0-99% inert gas preferably 10% methane : 90% inert gas is passed through a silica reactor heated in a furnace to 1000-1200 DEG C. to deposit a vitreous layer of carbon on the inside walls of the reactor. The inert gases may be any noble gas e.g. helium, neon or argon, or hydrogen and the reactor may be cylindrical, polygonal or conical in shape. The flow of methane is interrupted and silane vapour or vapour of a partially chlorinated silane, which may be diluted with hydrogen or argon, is passed through the reactor at 600-1200 DEG C. Trichloro silane is preferably employed at 900-1000 DEG C. When sufficient silicon has collected in the reactor it is allowed to cool to ambient temperature and the product removed. Vitreous carbon contaminating the silicon is removed by mechanical abrasion and/or immersion in an etching solution whereby carbon separates and floats off leaving pure silicon which is washed with aqueous HCl and dried. The reactor after washing and drying is ready for p re-use.
GB22874/57A 1956-07-26 1957-07-19 Process of producing pure silicon Expired GB820192A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US820192XA 1956-07-26 1956-07-26

Publications (1)

Publication Number Publication Date
GB820192A true GB820192A (en) 1959-09-16

Family

ID=22168512

Family Applications (1)

Application Number Title Priority Date Filing Date
GB22874/57A Expired GB820192A (en) 1956-07-26 1957-07-19 Process of producing pure silicon

Country Status (2)

Country Link
DE (1) DE1050321B (en)
GB (1) GB820192A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3069244A (en) * 1959-07-17 1962-12-18 Int Standard Electric Corp Production of silicon
CN102247933A (en) * 2011-03-22 2011-11-23 江西赛维Ldk太阳能高科技有限公司 Method for purifying silicon powder
CN102040222B (en) * 2009-10-23 2012-09-19 上海九晶电子材料股份有限公司 Method for separating silicon material from heavily doped silicon material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3069244A (en) * 1959-07-17 1962-12-18 Int Standard Electric Corp Production of silicon
CN102040222B (en) * 2009-10-23 2012-09-19 上海九晶电子材料股份有限公司 Method for separating silicon material from heavily doped silicon material
CN102247933A (en) * 2011-03-22 2011-11-23 江西赛维Ldk太阳能高科技有限公司 Method for purifying silicon powder

Also Published As

Publication number Publication date
DE1050321B (en) 1959-02-12

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