WO2011037473A1 - Method for producing high purity silicon - Google Patents

Method for producing high purity silicon Download PDF

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Publication number
WO2011037473A1
WO2011037473A1 PCT/NO2010/000332 NO2010000332W WO2011037473A1 WO 2011037473 A1 WO2011037473 A1 WO 2011037473A1 NO 2010000332 W NO2010000332 W NO 2010000332W WO 2011037473 A1 WO2011037473 A1 WO 2011037473A1
Authority
WO
WIPO (PCT)
Prior art keywords
silicon
leaching step
aqueous solution
heat treatment
calcium
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.)
Ceased
Application number
PCT/NO2010/000332
Other languages
English (en)
French (fr)
Inventor
Khalil Zeaiter
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.)
REC Solar AS
Original Assignee
Elkem Solar AS
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 Elkem Solar AS filed Critical Elkem Solar AS
Priority to BRPI1005443-0A priority Critical patent/BRPI1005443B1/pt
Priority to ES10819087.7T priority patent/ES2627503T3/es
Priority to CA2744802A priority patent/CA2744802C/en
Priority to IN1681DEN2012 priority patent/IN2012DN01681A/en
Priority to CN201080011131.XA priority patent/CN102369158B/zh
Priority to EP10819087.7A priority patent/EP2480497B1/en
Priority to US13/133,914 priority patent/US8920761B2/en
Publication of WO2011037473A1 publication Critical patent/WO2011037473A1/en
Anticipated expiration legal-status Critical
Ceased 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
    • C01B33/037—Purification
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates to a method for production of high purity silicon.
  • the main part of the calcium solidifies as a calcium-silicide phase along the grain boundaries of the silicon.
  • This calcium-silicide phase also contains a majority of other impurity elements contained in the metallurgical grade silicon, particularly iron, aluminium, titanium, vanadium, chromium and others.
  • the calcium-silicide phase containing these impurities dissolves during the leaching steps and the impurity elements contained in the calcium-silicide phase are thus removed from the silicon particles.
  • Very good results are obtained by the method of U.S. patent No. 4,539,194. It has, however, been found that not all calcium-silicide phase appears on the grain boundaries of the solidified silicon. Some of the calcium-silicide phase is isolated within the grains of silicon and in narrow channels and are consequently not available to the acid solutions during the leaching steps of U.S. patent No. 4,539,194.
  • the present invention thus relates to a method for producing high purity silicon comprising providing molten silicon containing 1-10% by weight of calcium, casting the molten silicon, crushing the silicon and subjecting the crushed silicon to a first leaching step in an aqueous solution of HCI and/or HCI + FeCI 3 and to a second leaching step in an aqueous solution of HF and HNO 3 , said method being characterized in that the leached silicon particles is subjected to heat treatment at a temperature of between 1250°C and 1420°C for a period of at least 20 minutes and subjecting the heat treated silicon to a third leaching step in an aqueous solution of HF and HNO 3 .
  • the heat treatment is carried out at a temperature of above 1300°C and more preferably at a temperature of above 1400°C.
  • the silicon particles is washed with water after the third leaching step.
  • the heat treatment can be carried out either as a batch process or continuously.
  • a continuous heat treatment can for instance be carried out in a tunnel furnace with a horizontal moving belt.
  • Samples of silicon particles having been alloyed by calcium and leached according to the method of U.S. patent No. 4,539,194 were heat treated for about 60 minutes at temperatures of 1250°C, 1400°C and 1420°C respectively and thereafter leached in an aqueous solution of HF + HN0 3 , and the resulting silicon particles where washed with water and dried.
  • Table 1 , 2 and 3 show the elemental analysis before heat treatment and after the HF+HNO 3 leaching as well as the reduction in percentage of impurity elements obtained by the process Table 1. Silicon particles heat treated at 1250°C and leached with HF+HNO3

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
PCT/NO2010/000332 2009-09-23 2010-09-09 Method for producing high purity silicon Ceased WO2011037473A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
BRPI1005443-0A BRPI1005443B1 (pt) 2009-09-23 2010-09-09 Método para a produção de silício de elevada pureza
ES10819087.7T ES2627503T3 (es) 2009-09-23 2010-09-09 Método para producir silicio de alta pureza
CA2744802A CA2744802C (en) 2009-09-23 2010-09-09 Method for producing high purity silicon
IN1681DEN2012 IN2012DN01681A (enExample) 2009-09-23 2010-09-09
CN201080011131.XA CN102369158B (zh) 2009-09-23 2010-09-09 生产高纯硅的方法
EP10819087.7A EP2480497B1 (en) 2009-09-23 2010-09-09 Method for producing high purity silicon
US13/133,914 US8920761B2 (en) 2009-09-23 2010-09-09 Method for producing high purity silicon

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20093054A NO331026B1 (no) 2009-09-23 2009-09-23 Fremgangsmate for fremstilling av hoyrent silisium
NO20093054 2009-09-23

Publications (1)

Publication Number Publication Date
WO2011037473A1 true WO2011037473A1 (en) 2011-03-31

Family

ID=43796046

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/NO2010/000332 Ceased WO2011037473A1 (en) 2009-09-23 2010-09-09 Method for producing high purity silicon

Country Status (10)

Country Link
US (1) US8920761B2 (enExample)
EP (1) EP2480497B1 (enExample)
CN (1) CN102369158B (enExample)
BR (1) BRPI1005443B1 (enExample)
CA (1) CA2744802C (enExample)
ES (1) ES2627503T3 (enExample)
IN (1) IN2012DN01681A (enExample)
MY (1) MY166519A (enExample)
NO (1) NO331026B1 (enExample)
WO (1) WO2011037473A1 (enExample)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102642838A (zh) * 2012-04-28 2012-08-22 中国科学院福建物质结构研究所 采用火法冶金与湿法冶金连用技术提纯高纯硅材料的方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI542544B (zh) 2012-06-25 2016-07-21 希利柯爾材料股份有限公司 純化矽之方法
EP2864252A1 (en) 2012-06-25 2015-04-29 Silicor Materials Inc. Method for purifying silicon
NO339608B1 (no) 2013-09-09 2017-01-09 Elkem Solar As Multikrystallinske silisiumingoter, silisiummasterlegering, fremgangsmåte for å øke utbyttet av multikrystallinske silisiumingoter for solceller
CN106629735B (zh) * 2016-12-09 2018-12-04 成都斯力康科技股份有限公司 一种适用于硅厂的智能控制配料分离系统
CN110508552A (zh) * 2019-09-27 2019-11-29 江苏美科硅能源有限公司 一种表面附氧化物的原生硅料的处理方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885364A (en) * 1955-05-31 1959-05-05 Columbia Broadcasting Syst Inc Method of treating semiconducting materials for electrical devices
US4379777A (en) * 1980-10-15 1983-04-12 Universite De Sherbrooke Purification of metallurgical grade silicon
US4539194A (en) * 1983-02-07 1985-09-03 Elkem A/S Method for production of pure silicon
US4643833A (en) * 1984-05-04 1987-02-17 Siemens Aktiengesellschaft Method for separating solid reaction products from silicon produced in an arc furnace
US4828814A (en) * 1985-03-13 1989-05-09 Sri International Process for purification of solid material
WO2001042136A1 (en) * 1999-12-08 2001-06-14 Elkem Asa Refining of metallurgical grade silicon

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1100218B (it) * 1978-11-09 1985-09-28 Montedison Spa Procedimento per la purificazione di silicio
CA1289333C (en) * 1986-03-07 1991-09-24 Angel Sanjurjo Process for purification of solid material
US5648042A (en) * 1995-10-10 1997-07-15 Centorr/Vacuum Industries, Inc High-temperature belt furnace apparatus and method of using same

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885364A (en) * 1955-05-31 1959-05-05 Columbia Broadcasting Syst Inc Method of treating semiconducting materials for electrical devices
US4379777A (en) * 1980-10-15 1983-04-12 Universite De Sherbrooke Purification of metallurgical grade silicon
US4539194A (en) * 1983-02-07 1985-09-03 Elkem A/S Method for production of pure silicon
US4643833A (en) * 1984-05-04 1987-02-17 Siemens Aktiengesellschaft Method for separating solid reaction products from silicon produced in an arc furnace
US4828814A (en) * 1985-03-13 1989-05-09 Sri International Process for purification of solid material
WO2001042136A1 (en) * 1999-12-08 2001-06-14 Elkem Asa Refining of metallurgical grade silicon

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2480497A4 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102642838A (zh) * 2012-04-28 2012-08-22 中国科学院福建物质结构研究所 采用火法冶金与湿法冶金连用技术提纯高纯硅材料的方法
CN102642838B (zh) * 2012-04-28 2014-10-15 中国科学院福建物质结构研究所 采用火法冶金与湿法冶金连用技术提纯高纯硅材料的方法

Also Published As

Publication number Publication date
BRPI1005443A2 (pt) 2016-03-08
CN102369158A (zh) 2012-03-07
NO20093054A1 (no) 2011-03-24
US8920761B2 (en) 2014-12-30
EP2480497A1 (en) 2012-08-01
CA2744802A1 (en) 2011-03-31
CA2744802C (en) 2017-01-03
BRPI1005443B1 (pt) 2020-08-11
CN102369158B (zh) 2014-05-14
IN2012DN01681A (enExample) 2015-06-05
EP2480497B1 (en) 2017-03-15
MY166519A (en) 2018-07-05
US20110250118A1 (en) 2011-10-13
NO331026B1 (no) 2011-09-12
EP2480497A4 (en) 2016-06-15
ES2627503T3 (es) 2017-07-28

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