JP4523274B2 - 高純度金属シリコンとその製錬法 - Google Patents
高純度金属シリコンとその製錬法 Download PDFInfo
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- JP4523274B2 JP4523274B2 JP2003518979A JP2003518979A JP4523274B2 JP 4523274 B2 JP4523274 B2 JP 4523274B2 JP 2003518979 A JP2003518979 A JP 2003518979A JP 2003518979 A JP2003518979 A JP 2003518979A JP 4523274 B2 JP4523274 B2 JP 4523274B2
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 105
- 239000010703 silicon Substances 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims description 27
- 238000003723 Smelting Methods 0.000 title claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000007670 refining Methods 0.000 claims abstract description 40
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000007711 solidification Methods 0.000 claims abstract description 16
- 230000008023 solidification Effects 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000460 chlorine Substances 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 238000012546 transfer Methods 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 238000004320 controlled atmosphere Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 18
- 238000005266 casting Methods 0.000 claims description 17
- 239000012535 impurity Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 230000006698 induction Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 31
- 229910052742 iron Inorganic materials 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000002844 melting Methods 0.000 abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 21
- 229910052796 boron Inorganic materials 0.000 description 21
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 18
- 229910052698 phosphorus Inorganic materials 0.000 description 18
- 239000011574 phosphorus Substances 0.000 description 18
- 239000007787 solid Substances 0.000 description 13
- 239000011575 calcium Substances 0.000 description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 11
- 229910052791 calcium Inorganic materials 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- 229910052719 titanium Inorganic materials 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 230000011514 reflex Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 229910021478 group 5 element Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Description
・高温の水素を使用するという難点、そのため、この方法を工業的に使用したときに、水素が漏洩することがあり、したがって、解決が困難な安全上の問題が生じる。
・生産性が低い、プラズマ下での溶融を実現するという難点。
・処理中にスラグを発生させる水素を使用するという難点、このスラグは精錬中の液体シリコンとプラズマ成分の間の障壁となり、それが精錬の反応速度を遅らせる。くわえて、このスラグは次第にるつぼの縁に集まり、液面に固形のスラグの環を形成するので、それをあとで除去する必要がある。作業を繰り返す内に、これらの度重なる除去工程がるつぼを損傷し、脆弱にし、その寿命を短くする。
トーチの陰極を構成する金属の気化によって該陰極が摩耗することで、形成されたプラズマが汚染されることになり、今度はそれがシリコンを汚染する。
・高温るつぼを備えた電気炉で、金属元素が500ppm未満の固体シリコンを中性雰囲気下で再溶融すること、
・プラズマ下での精錬を実現するために、高温るつぼを備えた電気炉内に溶融シリコンを移送すること、
・アルゴンと、塩素、フッ素、塩酸およびフッ化水素酸で構成されるグループのうちの少なくとも一つの気体との混合物をプラズマ発生気体として、プラズマ下で精錬すること、
・分離凝固が実現される鋳造鋳型内へ、制御雰囲気下で鋳込みをすること
ホウ素:0.5ppmから3ppm;リン/ホウ素は1と3の間;
不純物合計:100ppmから400ppm、
金属不純物合計:30ppmから300ppm、鉄:10ppmから200ppm、
炭素:10ppmから50ppm;酸素:50ppmから100ppm;
カルシウム:5ppmから30ppm;アルミニウム:5ppmから30ppm;チタン:2ppmから20ppm。
ホウ素:0.5ppmから2ppm;リン/ホウ素は1と3の間;
不純物合計:100ppmから250ppm、
金属不純物合計:30ppmから150ppm、鉄:10ppmから20ppm、
炭素:20ppmから30ppm;酸素:20ppmから50ppm;
カルシウム:5ppmから10ppm;アルミニウム:5ppmから10ppm;チタン:2ppmから5ppm。
鉄=0.24%;カルシウム:98ppm;アルミニウム:245ppm;チタン:240ppm;ホウ素:32ppm;リン:19ppm;炭素:100ppm;酸素:1200ppm。
鉄=285ppm;カルシウム:24ppm;アルミニウム:14ppm;チタン:9ppm;ホウ素28ppm;リン:10ppm;炭素:100ppm;酸素:800ppm。
鉄=280ppm;カルシウム:23ppm;アルミニウム:14ppm;チタン:9ppm;ホウ素3ppm;リン:8ppm;炭素:50ppm;酸素:80ppm。
鉄=160ppm;カルシウム:9ppm;アルミニウム:8ppm;チタン:5ppm;ホウ素3ppm;リン:8ppm;炭素:50ppm;酸素:90ppm。
鉄=0.25%;カルシウム:90ppm;アルミニウム:210ppm;チタン:240ppm;ホウ素32ppm;リン:20ppm;炭素:100ppm;酸素:400ppm。
鉄=95ppm;カルシウム:23ppm;アルミニウム:12ppm;チタン:9ppm;ホウ素32ppm;リン:6ppm;炭素:100ppm;酸素:400ppm。
鉄=85ppm;カルシウム:23ppm;アルミニウム:12ppm;チタン:9ppm;ホウ素2ppm;リン:5ppm;炭素:30ppm;酸素:50ppm。
鉄=16ppm;カルシウム:9ppm;アルミニウム:7ppm;チタン:4ppm;ホウ素2ppm;リン:5ppm;炭素:30ppm;酸素:50ppm。
Claims (13)
- 酸素又は塩素で精錬され金属元素を500ppm未満含有する金属シリコンから光起電力品位のシリコンを製錬する方法であって、以下を有する方法:
・高温るつぼを備えた電気炉で、中性雰囲気下で、精錬シリコンを再溶融すること、
・プラズマ下で精錬を実現するために、高温るつぼを備えた電気炉内に溶融シリコンを輸送すること、
・アルゴンと、塩素、フッ素、塩酸およびフッ化水素酸で構成されるグループに属する少なくとも一つの気体との混合物をプラズマ発生気体とし、該混合物が5%から90%のアルゴンを含有する状態で、再溶融シリコンをプラズマ下で精錬すること、
・分離凝固が実現される鋳造鋳型内へ、制御雰囲気下で鋳込みをすること。 - 金属元素が500ppm未満であるシリコンの調製が、液体分画内の金属不純物を濃縮するように、分離凝固によって行われることを特徴とする、請求項1に記載の方法。
- 再溶融が連続するロットごとに行われることを特徴とする、請求項1又は請求項2に記載の方法。
- シリコンの再溶融およびプラズマ下での精錬が、二つの異なる作業施設で実現されることを特徴とする、請求項1から請求項3のいずれか一つに記載の方法。
- 再溶融とプラズマ下での精錬との間のシリコンの輸送が、炉のフレーム、インダクタ、るつぼおよび液体シリコンによって構成されるユニットの移動による移し換えなしに行われることを特徴とする、請求項1から請求項4のいずれか一つに記載の方法。
- プラズマ下での精錬が、アルゴンを50%から70%含有するHF−アルゴンおよび/又はHCl−アルゴン気体混合物によって実現されることを特徴とする、請求項1から請求項5のいずれか一つに記載の方法。
- プラズマ源が、周波数が100kHzと4MHzの間に含まれる電源から給電される誘導トーチであることを特徴とする、請求項1から請求項6のいずれか一つに記載の方法。
- プラズマ精錬前の最初の分離凝固が、2×10-5m/s未満の凝固先頭の前進速度で実施されることを特徴とする、請求項2から請求項7のいずれか一つに記載の方法。
- プラズマ精錬後の分離凝固が、10-5m/s未満の凝固先頭の前進速度で実施されることを特徴とする、請求項1から請求項8のいずれか一つに記載の方法。
- プラズマ精錬後の分離凝固先頭の前進速度が5×10-6m/s未満であることを特徴とする、請求項9に記載の方法。
- 分離凝固作業が反射炉内で行われることを特徴とする、請求項1から請求項10のいずれか一つに記載の方法。
- シリコンの再溶融とプラズマ精錬のために使用される電気炉が誘導加熱炉であることを特徴とする、請求項1から請求項11のいずれか一つに記載の方法。
- シリコンの再溶融とプラズマ精錬のために使用される電気炉が、シリカ製、炭素製又は炭化ケイ素製であることを特徴とする、請求項1から請求項12のいずれか一つに記載の方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0109788A FR2827592B1 (fr) | 2001-07-23 | 2001-07-23 | Silicium metallurgique de haute purete et procede d'elaboration |
PCT/FR2002/002602 WO2003014019A1 (fr) | 2001-07-23 | 2002-07-22 | Silicium metallurgique de haute purete et procede d'elaboration |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2004537491A JP2004537491A (ja) | 2004-12-16 |
JP4523274B2 true JP4523274B2 (ja) | 2010-08-11 |
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Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
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JP2003515451A Expired - Fee Related JP4410847B2 (ja) | 2001-07-23 | 2002-07-22 | 中純度金属シリコンとその製錬法 |
JP2003518979A Expired - Fee Related JP4523274B2 (ja) | 2001-07-23 | 2002-07-22 | 高純度金属シリコンとその製錬法 |
Family Applications Before (1)
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JP2003515451A Expired - Fee Related JP4410847B2 (ja) | 2001-07-23 | 2002-07-22 | 中純度金属シリコンとその製錬法 |
Country Status (12)
Country | Link |
---|---|
US (2) | US7404941B2 (ja) |
EP (2) | EP1409406B1 (ja) |
JP (2) | JP4410847B2 (ja) |
CN (2) | CN1295147C (ja) |
AT (2) | ATE382581T1 (ja) |
BR (2) | BR0211195B1 (ja) |
DE (2) | DE60224394T2 (ja) |
ES (2) | ES2357501T3 (ja) |
FR (1) | FR2827592B1 (ja) |
NO (2) | NO335985B1 (ja) |
WO (2) | WO2003010090A1 (ja) |
ZA (2) | ZA200400276B (ja) |
Families Citing this family (40)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NO333319B1 (no) * | 2003-12-29 | 2013-05-06 | Elkem As | Silisiummateriale for fremstilling av solceller |
FR2869028B1 (fr) * | 2004-04-20 | 2006-07-07 | Efd Induction Sa Sa | Procede et installation de fabrication de blocs d'un materiau semiconducteur |
JP4749730B2 (ja) * | 2005-02-09 | 2011-08-17 | 新日鉄マテリアルズ株式会社 | Siの精錬方法 |
MX2008011655A (es) * | 2006-03-15 | 2009-01-14 | Resc Invest Llc | Metodo para hacer silicio para celdas solares y otras aplicaciones. |
ES2497990T3 (es) * | 2006-04-04 | 2014-09-23 | Silicor Materials Inc. | Método para purificar silicio |
US7682585B2 (en) * | 2006-04-25 | 2010-03-23 | The Arizona Board Of Regents On Behalf Of The University Of Arizona | Silicon refining process |
DE102006034061A1 (de) * | 2006-07-20 | 2008-01-24 | REV Renewable Energy Ventures, Inc., Aloha | Polysilanverarbeitung und Verwendung |
US7955583B2 (en) * | 2006-08-31 | 2011-06-07 | Mitsubishi Materials Corporation | Metallic silicon and method for manufacturing the same |
AU2007295860A1 (en) * | 2006-09-14 | 2008-03-20 | Silicium Becancour Inc. | Process and apparatus for purifying low-grade silicon material |
JP5210167B2 (ja) * | 2006-09-29 | 2013-06-12 | 信越化学工業株式会社 | 珪素の精製方法 |
FR2908125B1 (fr) | 2006-11-02 | 2009-11-20 | Commissariat Energie Atomique | Procede de purification de silicium metallurgique par solidification dirigee |
CN100460320C (zh) * | 2007-03-08 | 2009-02-11 | 陈应天 | 使用自旋仰角跟踪的太阳炉对材料进行真空提纯的方法 |
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