DE1213627B - Verfahren zur Raffination von unreinem Silicium und Germanium durch Schmelzflusselektrolyse - Google Patents
Verfahren zur Raffination von unreinem Silicium und Germanium durch SchmelzflusselektrolyseInfo
- Publication number
- DE1213627B DE1213627B DEG37274A DEG0037274A DE1213627B DE 1213627 B DE1213627 B DE 1213627B DE G37274 A DEG37274 A DE G37274A DE G0037274 A DEG0037274 A DE G0037274A DE 1213627 B DE1213627 B DE 1213627B
- Authority
- DE
- Germany
- Prior art keywords
- silicon
- anode
- germanium
- electrolyte
- temperature
- 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.)
- Pending
Links
- 239000010703 silicon Substances 0.000 title claims description 56
- 229910052710 silicon Inorganic materials 0.000 title claims description 55
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims description 32
- 229910052732 germanium Inorganic materials 0.000 title claims description 31
- 238000000034 method Methods 0.000 title claims description 22
- 238000005868 electrolysis reaction Methods 0.000 title claims description 15
- 238000007670 refining Methods 0.000 title claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 56
- 239000003792 electrolyte Substances 0.000 claims description 42
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- 229910000676 Si alloy Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001610 cryolite Inorganic materials 0.000 claims description 5
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims 1
- 239000013589 supplement Substances 0.000 claims 1
- 210000004027 cell Anatomy 0.000 description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 30
- 229910002804 graphite Inorganic materials 0.000 description 21
- 239000010439 graphite Substances 0.000 description 21
- 229910052799 carbon Inorganic materials 0.000 description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 9
- 229910010271 silicon carbide Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 150000002222 fluorine compounds Chemical class 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910002065 alloy metal Inorganic materials 0.000 description 3
- 210000002421 cell wall Anatomy 0.000 description 3
- 150000001805 chlorine compounds Chemical class 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 229910000927 Ge alloy Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical class Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B41/00—Obtaining germanium
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/33—Silicon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Electrolytic Production Of Metals (AREA)
- Silicon Compounds (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US179726A US3219561A (en) | 1962-03-14 | 1962-03-14 | Dual cell refining of silicon and germanium |
| US179725A US3254010A (en) | 1962-03-14 | 1962-03-14 | Refining of silicon and germanium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1213627B true DE1213627B (de) | 1966-03-31 |
Family
ID=26875592
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEG37274A Pending DE1213627B (de) | 1962-03-14 | 1963-03-14 | Verfahren zur Raffination von unreinem Silicium und Germanium durch Schmelzflusselektrolyse |
| DEG37275A Pending DE1217077B (de) | 1962-03-14 | 1963-03-14 | Verfahren und Vorrichtung zur Herstellung von Silicium oder Germanium hoher Reinheit durch Schmelzflusselektrolyse |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEG37275A Pending DE1217077B (de) | 1962-03-14 | 1963-03-14 | Verfahren und Vorrichtung zur Herstellung von Silicium oder Germanium hoher Reinheit durch Schmelzflusselektrolyse |
Country Status (5)
| Country | Link |
|---|---|
| US (2) | US3219561A (enrdf_load_stackoverflow) |
| CH (2) | CH410441A (enrdf_load_stackoverflow) |
| DE (2) | DE1213627B (enrdf_load_stackoverflow) |
| GB (2) | GB989452A (enrdf_load_stackoverflow) |
| NL (2) | NL290208A (enrdf_load_stackoverflow) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH426279A (fr) * | 1965-06-15 | 1966-12-15 | Fiduciaire Generale S A | Cellule électrolytique pour la fabrication de silicium |
| US3983012A (en) * | 1975-10-08 | 1976-09-28 | The Board Of Trustees Of Leland Stanford Junior University | Epitaxial growth of silicon or germanium by electrodeposition from molten salts |
| US4142947A (en) * | 1977-05-12 | 1979-03-06 | Uri Cohen | Electrodeposition of polycrystalline silicon from a molten fluoride bath and product |
| FR2480796A1 (fr) * | 1980-04-21 | 1981-10-23 | Extramet Sarl | Procede de production de silicium de haute purete par voie electrochimique |
| US4448651A (en) * | 1982-06-10 | 1984-05-15 | The United States Of America As Represented By The United States Department Of Energy | Process for producing silicon |
| NO156172C (no) * | 1984-02-13 | 1987-08-12 | Ila Lilleby Smelteverker | Fremgangsmaate til fremstilling av renset silisium ved elektrolytisk raffinering. |
| NO20063072L (no) * | 2006-03-10 | 2007-09-11 | Elkem As | Fremgangsmate for elektrolytisk raffinering av metaller |
| US7901561B2 (en) * | 2006-03-10 | 2011-03-08 | Elkem As | Method for electrolytic production and refining of metals |
| ES2633113T3 (es) | 2006-03-10 | 2017-09-19 | Elkem As | Método para la producción y refinado electrolítico de silicio |
| CN101743342A (zh) | 2007-06-18 | 2010-06-16 | Rec斯坎沃佛股份有限公司 | 从切割剩余物回收元素硅的方法 |
| US8460535B2 (en) | 2009-04-30 | 2013-06-11 | Infinium, Inc. | Primary production of elements |
| US20120132034A1 (en) * | 2009-05-26 | 2012-05-31 | Sumitomo Chemical Company, Limited | Process for producing refined metal or metalloid |
| WO2012083480A1 (en) * | 2010-12-20 | 2012-06-28 | Epro Development Limited | Method and apparatus for producing pure silicon |
| CN103243385B (zh) * | 2013-05-13 | 2016-04-27 | 北京科技大学 | 电解精炼-液态阴极原位定向凝固制备高纯单晶硅的方法 |
| CN110482556B (zh) * | 2019-09-10 | 2020-12-08 | 中国科学院合肥物质科学研究院 | 一种用于硅材料低温精炼除硼的造渣剂及其使用方法 |
| CN112708764A (zh) * | 2020-12-15 | 2021-04-27 | 湖南腾驰环保科技有限公司 | 一种从铜锗合金物料中综合回收二氧化锗和铜的方法 |
| CN115305507B (zh) * | 2021-05-08 | 2024-09-03 | 中南大学 | 熔盐电解氧化铝生产金属铝的方法 |
| CN115305568A (zh) * | 2021-05-08 | 2022-11-08 | 中南大学 | 一种多晶硅的冶炼方法 |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE533780A (enrdf_load_stackoverflow) * | ||||
| US800984A (en) * | 1905-06-02 | 1905-10-03 | Henry M Chance | Process of purifying metals. |
| US2755240A (en) * | 1953-11-02 | 1956-07-17 | Shawinigan Water And Power Com | Electrolysis of titanium tetrachloride to produce titanium |
| US3009870A (en) * | 1954-05-25 | 1961-11-21 | Ver Aluminum Werke | Electrolytic cell |
| GB833767A (en) * | 1956-10-19 | 1960-04-27 | Timax Corp | Continuous electrolytic production of titanium |
| US2952605A (en) * | 1956-12-29 | 1960-09-13 | Montedison Spa | Refractories resistant to aggressive melts and treatment for obtaining them |
| US2892763A (en) * | 1957-04-12 | 1959-06-30 | American Potash & Chem Corp | Production of pure elemental silicon |
| US2940911A (en) * | 1959-01-02 | 1960-06-14 | American Potash & Chem Corp | Electrorefining of elemental boron |
| US3030284A (en) * | 1960-11-03 | 1962-04-17 | American Potash & Chem Corp | Electrolytic production of elemental boron |
-
0
- NL NL290209D patent/NL290209A/xx unknown
- NL NL290208D patent/NL290208A/xx unknown
-
1962
- 1962-03-14 US US179726A patent/US3219561A/en not_active Expired - Lifetime
- 1962-03-14 US US179725A patent/US3254010A/en not_active Expired - Lifetime
-
1963
- 1963-03-08 GB GB9362/63A patent/GB989452A/en not_active Expired
- 1963-03-08 GB GB9363/63A patent/GB993192A/en not_active Expired
- 1963-03-12 CH CH314563A patent/CH410441A/fr unknown
- 1963-03-13 CH CH319963A patent/CH409416A/fr unknown
- 1963-03-14 DE DEG37274A patent/DE1213627B/de active Pending
- 1963-03-14 DE DEG37275A patent/DE1217077B/de active Pending
Non-Patent Citations (1)
| Title |
|---|
| None * |
Also Published As
| Publication number | Publication date |
|---|---|
| CH410441A (fr) | 1966-03-31 |
| GB989452A (en) | 1965-04-22 |
| US3254010A (en) | 1966-05-31 |
| US3219561A (en) | 1965-11-23 |
| GB993192A (en) | 1965-05-26 |
| CH409416A (fr) | 1966-03-15 |
| DE1217077B (de) | 1966-05-18 |
| NL290208A (enrdf_load_stackoverflow) | |
| NL290209A (enrdf_load_stackoverflow) |
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