GB745698A - Improvements in or relating to methods of producing silicon of high purity - Google Patents

Improvements in or relating to methods of producing silicon of high purity

Info

Publication number
GB745698A
GB745698A GB26446/53A GB2644653A GB745698A GB 745698 A GB745698 A GB 745698A GB 26446/53 A GB26446/53 A GB 26446/53A GB 2644653 A GB2644653 A GB 2644653A GB 745698 A GB745698 A GB 745698A
Authority
GB
United Kingdom
Prior art keywords
pure
silane
silicon
silicon tetrachloride
decomposition
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
GB26446/53A
Inventor
Jack Mccreath Wilson
Jack Augustus Radley
Eileen Dulcie Neale
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.)
STC PLC
Original Assignee
Standard Telephone and Cables PLC
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
Priority to BE561654D priority Critical patent/BE561654A/xx
Priority to BE565604D priority patent/BE565604A/xx
Priority to BE561650D priority patent/BE561650A/xx
Priority to NL112548D priority patent/NL112548C/xx
Priority to BE532054D priority patent/BE532054A/xx
Priority to FR75903D priority patent/FR75903E/fr
Priority to NL225733D priority patent/NL225733A/xx
Priority to GB26446/53A priority patent/GB745698A/en
Application filed by Standard Telephone and Cables PLC filed Critical Standard Telephone and Cables PLC
Priority to DEI9153A priority patent/DE1042553B/en
Priority to FR1108543D priority patent/FR1108543A/en
Priority to CH1063854A priority patent/CH370751A/en
Priority to FR67266D priority patent/FR67266E/en
Publication of GB745698A publication Critical patent/GB745698A/en
Priority to FR70026D priority patent/FR70026E/en
Priority to GB31424/56A priority patent/GB829422A/en
Priority to FR749492A priority patent/FR72742E/en
Priority to FR749491A priority patent/FR72741E/en
Priority to FR72288D priority patent/FR72288E/en
Priority to US716652A priority patent/US2987139A/en
Priority to DEI14512A priority patent/DE1065389B/en
Priority to FR760198A priority patent/FR73392E/en
Priority to CH5687258A priority patent/CH373741A/en
Priority to FR769353A priority patent/FR73946E/en
Priority to FR771605A priority patent/FR74454E/en
Priority to FR783396A priority patent/FR75047E/en
Priority to FR790410A priority patent/FR75654E/en
Priority to FR794679A priority patent/FR75905E/en
Priority to BE663513D priority patent/BE663513A/nl
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Compounds (AREA)

Abstract

<PICT:0745698/III/1> Pure silicon is prepared by the thermal decomposition of silane (SiH4) by heating to temperatures between the decomposition temperature (about 500 DEG C.) and 800 DEG C. and with molecular concentrations about 0.3 per cent. The silane may be decomposed so as to form a coherent body around a seed of pure silicon. In Fig. 2 pure silane, preheated by heater 28, is drawn through aperture 27 via valve 25 and flow meter 24 into decomposition chamber 12 by a vacuum pump connected to outlet 29. The gas flow is directed on to the silicon seed 16 supported on rod 17 and heated by copper current concentrator 18, itself cooled by water in coil 19, and primary coil 22 which form the tuned circuit of an induction heater (see Group XI). The rod 17 passes through a vacuum seal 31 and is connected to a mechanism 32 which alters its position so as to give optimum crystal growth. Pure silane is prepared from silicon tetrachloride and lithium aluminium hydride. Silicon tetrachloride is refluxed with copper turnings and the arsenic content reduced to less than 0.01 micrograms per mililitre by fractional distillation of the chloride. The silicon tetrachloride is then mixed with pure dry ether or tetrahydrofuran, and reacted with lithium aluminium hydride which has also been refluxed with pure dry ether or tetrahydrofuran. The resulting silane after fractional freezing and distillation may be stored in cylinders or swept straight into the decomposition chamber with an inert gas.
GB26446/53A 1953-09-25 1953-09-25 Improvements in or relating to methods of producing silicon of high purity Expired GB745698A (en)

Priority Applications (27)

Application Number Priority Date Filing Date Title
NL225733D NL225733A (en) 1953-09-25
BE561650D BE561650A (en) 1953-09-25
NL112548D NL112548C (en) 1953-09-25
BE532054D BE532054A (en) 1953-09-25
FR75903D FR75903E (en) 1953-09-25
BE561654D BE561654A (en) 1953-09-25
BE565604D BE565604A (en) 1953-09-25
GB26446/53A GB745698A (en) 1953-09-25 1953-09-25 Improvements in or relating to methods of producing silicon of high purity
DEI9153A DE1042553B (en) 1953-09-25 1954-09-18 Process for the production of high purity silicon
FR1108543D FR1108543A (en) 1953-09-25 1954-09-23 High purity silicon production method
CH1063854A CH370751A (en) 1953-09-25 1954-09-25 Process for the production of a coherent body consisting of a highly pure chemical element for semiconductor technology
FR67266D FR67266E (en) 1953-09-25 1954-09-29 High purity silicon production method
FR70026D FR70026E (en) 1953-09-25 1956-08-14 High purity silicon production method
GB31424/56A GB829422A (en) 1953-09-25 1956-10-16 Method and apparatus for producing semi-conductor materials of high purity
FR749492A FR72742E (en) 1953-09-25 1957-10-15 High purity silicon production method
FR72288D FR72288E (en) 1953-09-25 1957-10-15 High purity silicon production method
FR749491A FR72741E (en) 1953-09-25 1957-10-15 High purity silicon production method
US716652A US2987139A (en) 1953-09-25 1958-02-21 Manufacture of pure silicon
DEI14512A DE1065389B (en) 1953-09-25 1958-03-06 Process for purifying silicon hydride to produce extremely pure silicon for semiconductor use
FR760198A FR73392E (en) 1953-09-25 1958-03-11 High purity silicon production method
CH5687258A CH373741A (en) 1953-09-25 1958-03-12 Process for purifying silane
FR769353A FR73946E (en) 1953-09-25 1958-07-02 High purity silicon production method
FR771605A FR74454E (en) 1953-09-25 1958-07-31 High purity silicon production method
FR783396A FR75047E (en) 1953-09-25 1959-01-06 High purity silicon production method
FR790410A FR75654E (en) 1953-09-25 1959-03-24 High purity silicon production method
FR794679A FR75905E (en) 1953-09-25 1959-05-14 High purity silicon production method
BE663513D BE663513A (en) 1953-09-25 1965-05-06

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB26446/53A GB745698A (en) 1953-09-25 1953-09-25 Improvements in or relating to methods of producing silicon of high purity

Publications (1)

Publication Number Publication Date
GB745698A true GB745698A (en) 1956-02-29

Family

ID=10243739

Family Applications (1)

Application Number Title Priority Date Filing Date
GB26446/53A Expired GB745698A (en) 1953-09-25 1953-09-25 Improvements in or relating to methods of producing silicon of high purity

Country Status (1)

Country Link
GB (1) GB745698A (en)

Cited By (34)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2888328A (en) * 1955-08-16 1959-05-26 Int Standard Electric Corp Methods of producing silicon of high purity
US2931709A (en) * 1956-09-17 1960-04-05 Robert S Aries Decarburizing silicon tetrachloride
DE1082883B (en) * 1958-06-25 1960-06-09 Wacker Chemie Gmbh Process for the production of high purity boron, silicon or germanium or mixtures of these substances
US2943918A (en) * 1956-02-11 1960-07-05 Pechiney Prod Chimiques Sa Process for manufacturing dense, extra pure silicon
DE1095261B (en) * 1958-03-21 1960-12-22 Int Standard Electric Corp Process for the production of semiconductor elements of high purity by thermal decomposition of the hydrides
US2987139A (en) * 1953-09-25 1961-06-06 Int Standard Electric Corp Manufacture of pure silicon
US2988427A (en) * 1957-07-17 1961-06-13 Kali Chemie Ag Method for the purification of hydrides of silicon and germanium group of the periodic system
US2989378A (en) * 1956-10-16 1961-06-20 Int Standard Electric Corp Producing silicon of high purity
US2993762A (en) * 1956-10-16 1961-07-25 Int Standard Electric Corp Methods of producing silicon of high purity
US2993763A (en) * 1957-11-14 1961-07-25 Plessey Co Ltd Manufacturing process for the preparation of flakes of sintered silicon
US3000768A (en) * 1959-05-28 1961-09-19 Ibm Semiconductor device with controlled zone thickness
US3006734A (en) * 1957-11-14 1961-10-31 Plessey Co Ltd Process for preparing pure silicon
US3011877A (en) * 1956-06-25 1961-12-05 Siemens Ag Production of high-purity semiconductor materials for electrical purposes
US3016289A (en) * 1957-04-25 1962-01-09 Licentia Gmbh Process for producing purified silicon halogenide
US3019087A (en) * 1958-09-29 1962-01-30 Merck & Co Inc Purification of silane
US3023087A (en) * 1957-09-07 1962-02-27 Wacker Chemie Gmbh Process for the production of extremely pure silicon
US3029135A (en) * 1958-05-16 1962-04-10 Int Standard Electric Corp Purification of gases used in the production of silicon
US3030189A (en) * 1958-05-19 1962-04-17 Siemens Ag Methods of producing substances of highest purity, particularly electric semiconductors
DE1128412B (en) * 1959-12-17 1962-04-26 Metallgesellschaft Ag Process for the production of hyperpure silicon by the thermal decomposition of gaseous silicon compounds
US3051557A (en) * 1958-03-12 1962-08-28 Int Standard Electric Corp Manufacture of pure silicon
US3053631A (en) * 1956-08-04 1962-09-11 Int Standard Electric Corp Methods of producing silicon of high purity
US3055741A (en) * 1960-12-22 1962-09-25 Sylvania Electric Prod Method for producing silicon
US3069244A (en) * 1959-07-17 1962-12-18 Int Standard Electric Corp Production of silicon
US3078150A (en) * 1958-05-14 1963-02-19 Int Standard Electric Corp Production of semi-conductor materials
US3092462A (en) * 1960-01-28 1963-06-04 Philips Corp Method for the manufacture of rods of meltable material
US3095279A (en) * 1960-04-07 1963-06-25 Tung Sol Electric Inc Apparatus for producing pure silicon
US3126248A (en) * 1964-03-24 Process for producing purified
US3128154A (en) * 1958-12-19 1964-04-07 Eagle Picher Co Process for producing crystalline silicon over a substrate and removal therefrom
US3177100A (en) * 1963-09-09 1965-04-06 Rca Corp Depositing epitaxial layer of silicon from a vapor mixture of sih4 and h3
US3192072A (en) * 1960-12-08 1965-06-29 Slemens & Halske Ag Method of pulling a dendritic crystal from a vapor atmosphere
DE1216842B (en) * 1960-09-30 1966-05-18 Karl Ernst Hoffmann Process for the production of the purest silicon and germanium
EP0112385A1 (en) * 1982-06-22 1984-07-04 Harry Levin Apparatus and process for making solar grade silicon.
EP1400490A1 (en) * 2002-09-17 2004-03-24 Degussa AG Deposition of a solid by thermal decomposition of a gaseous substance in a bowl reactor
US8414863B2 (en) 2006-07-25 2013-04-09 Spawnt Private S.A.R.L. Hydrogen and energy generation by thermal conversion of silanes

Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3126248A (en) * 1964-03-24 Process for producing purified
US2987139A (en) * 1953-09-25 1961-06-06 Int Standard Electric Corp Manufacture of pure silicon
US2888328A (en) * 1955-08-16 1959-05-26 Int Standard Electric Corp Methods of producing silicon of high purity
US2943918A (en) * 1956-02-11 1960-07-05 Pechiney Prod Chimiques Sa Process for manufacturing dense, extra pure silicon
US3011877A (en) * 1956-06-25 1961-12-05 Siemens Ag Production of high-purity semiconductor materials for electrical purposes
US3053631A (en) * 1956-08-04 1962-09-11 Int Standard Electric Corp Methods of producing silicon of high purity
US2931709A (en) * 1956-09-17 1960-04-05 Robert S Aries Decarburizing silicon tetrachloride
US2993762A (en) * 1956-10-16 1961-07-25 Int Standard Electric Corp Methods of producing silicon of high purity
US2989378A (en) * 1956-10-16 1961-06-20 Int Standard Electric Corp Producing silicon of high purity
US3016289A (en) * 1957-04-25 1962-01-09 Licentia Gmbh Process for producing purified silicon halogenide
US2988427A (en) * 1957-07-17 1961-06-13 Kali Chemie Ag Method for the purification of hydrides of silicon and germanium group of the periodic system
US3023087A (en) * 1957-09-07 1962-02-27 Wacker Chemie Gmbh Process for the production of extremely pure silicon
US2993763A (en) * 1957-11-14 1961-07-25 Plessey Co Ltd Manufacturing process for the preparation of flakes of sintered silicon
US3006734A (en) * 1957-11-14 1961-10-31 Plessey Co Ltd Process for preparing pure silicon
US3051557A (en) * 1958-03-12 1962-08-28 Int Standard Electric Corp Manufacture of pure silicon
DE1095261B (en) * 1958-03-21 1960-12-22 Int Standard Electric Corp Process for the production of semiconductor elements of high purity by thermal decomposition of the hydrides
US3078150A (en) * 1958-05-14 1963-02-19 Int Standard Electric Corp Production of semi-conductor materials
US3029135A (en) * 1958-05-16 1962-04-10 Int Standard Electric Corp Purification of gases used in the production of silicon
US3030189A (en) * 1958-05-19 1962-04-17 Siemens Ag Methods of producing substances of highest purity, particularly electric semiconductors
DE1082883B (en) * 1958-06-25 1960-06-09 Wacker Chemie Gmbh Process for the production of high purity boron, silicon or germanium or mixtures of these substances
US3019087A (en) * 1958-09-29 1962-01-30 Merck & Co Inc Purification of silane
US3128154A (en) * 1958-12-19 1964-04-07 Eagle Picher Co Process for producing crystalline silicon over a substrate and removal therefrom
US3000768A (en) * 1959-05-28 1961-09-19 Ibm Semiconductor device with controlled zone thickness
US3069244A (en) * 1959-07-17 1962-12-18 Int Standard Electric Corp Production of silicon
DE1128412B (en) * 1959-12-17 1962-04-26 Metallgesellschaft Ag Process for the production of hyperpure silicon by the thermal decomposition of gaseous silicon compounds
US3092462A (en) * 1960-01-28 1963-06-04 Philips Corp Method for the manufacture of rods of meltable material
US3095279A (en) * 1960-04-07 1963-06-25 Tung Sol Electric Inc Apparatus for producing pure silicon
DE1216842B (en) * 1960-09-30 1966-05-18 Karl Ernst Hoffmann Process for the production of the purest silicon and germanium
US3192072A (en) * 1960-12-08 1965-06-29 Slemens & Halske Ag Method of pulling a dendritic crystal from a vapor atmosphere
US3055741A (en) * 1960-12-22 1962-09-25 Sylvania Electric Prod Method for producing silicon
US3177100A (en) * 1963-09-09 1965-04-06 Rca Corp Depositing epitaxial layer of silicon from a vapor mixture of sih4 and h3
EP0112385A1 (en) * 1982-06-22 1984-07-04 Harry Levin Apparatus and process for making solar grade silicon.
EP0112385A4 (en) * 1982-06-22 1984-11-20 Harry Levin Apparatus and process for making solar grade silicon.
EP1400490A1 (en) * 2002-09-17 2004-03-24 Degussa AG Deposition of a solid by thermal decomposition of a gaseous substance in a bowl reactor
US8414863B2 (en) 2006-07-25 2013-04-09 Spawnt Private S.A.R.L. Hydrogen and energy generation by thermal conversion of silanes

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