CN1231416C - 冶金级硅的纯化方法 - Google Patents
冶金级硅的纯化方法 Download PDFInfo
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- CN1231416C CN1231416C CNB008169047A CN00816904A CN1231416C CN 1231416 C CN1231416 C CN 1231416C CN B008169047 A CNB008169047 A CN B008169047A CN 00816904 A CN00816904 A CN 00816904A CN 1231416 C CN1231416 C CN 1231416C
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 64
- 239000010703 silicon Substances 0.000 title claims abstract description 64
- 238000007670 refining Methods 0.000 title description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000011575 calcium Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 239000004411 aluminium Substances 0.000 claims description 13
- 238000003723 Smelting Methods 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 20
- 239000000956 alloy Substances 0.000 description 20
- 239000012535 impurity Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000000243 solution 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
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/547—Monocrystalline silicon PV cells
-
- 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
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
本发明涉及一种纯化冶金级硅的方法,其中将含钙的化合物在硅从熔炉放出之前或之后加到熔融硅中。在较高的冷却速率下铸造硅和使其固化,将固化的硅碾碎,并使其经受由两个浸提步骤组成的纯化过程。在第一个浸提步骤中,硅用FeCl3或FeCl3和HCl的水溶液处理,使硅分解,在第二个浸提步骤中硅用HF或HF/HNO3的水溶液处理。加入到熔融硅中的含钙化合物的量必须提供熔融硅中0.3-0.95%重量的钙,和熔融硅中铝和铁的重量比通过加铝到熔融硅中控制在0.5-2.0。
Description
发明领域
本发明涉及从冶金级硅生产高纯硅的方法。
背景技术
冶金级硅含有某些金属和非金属杂质,这些杂质使冶金级硅不适宜用于太阳能电池。非金属杂质如硼和磷主要通过选择适当的生产硅金属的原料可被减少,但该法对于最重要的金属杂质铁、铝、锰、铜和镍等而言仅能减少到一定程度。可是高纯度的原料极昂贵,因此希望设法获得一种简单而便宜的纯化方法,通过该法可将金属杂质除去和/或减少到如此低的程度,以使精制硅适于生产太阳能电池。
已知许多金属杂质是在硅金属结晶期间排出的,而且这些杂质将沿着硅的晶粒边界结晶,或是作为金属间化合物或作为硅化物。尤其是铁和铝属于这种情况。因此硅的纯化可以通过如此进行结晶来完成,以使这些杂质可被集中和除去,例如用晶体拉伸、区域熔融或类似的方法,或通过应用一种不浸蚀硅金属的酸把杂质溶解。
晶体拉伸以及区域熔融是很有效的纯化方法,但极其昂贵,并且在得到令人满意的太阳能电池质量之前需要至少两次纯化冶金级硅。
由US No.4,539,194可知一种方法,其中熔融的硅与1-10%重量的钙熔合,然后固化的合金以两个步骤浸提。在第一个浸提步骤中,是应用一种FeCl3和HCl的水溶液,该溶液把硅分解为小的硅颗粒。在第二个浸提步骤中,是应用一种HF和HNO3的水溶液。通过这一方法,对于铁和铝二者得到了充分的纯化,而且对于磷也得到了某种程度的纯化。然而,US No.4,539,194的方法有某些缺陷。例如较大量的钙加到硅中是昂贵的,因为在熔合期间钙的损失高并随着硅中钙量的增加而增加。此外,在两个浸提步骤中控制浸提反应是困难的,因为硅烷和H2气体的反应是高放热的可引起自然和爆炸。最后,硅中高量的钙招致极细颗粒硅形式硅的高损失,这是在两个浸提步骤后进行的清洗步骤中损失的。
发明公开
现已令人惊异地发现,通过加入较少量的钙可得到良好的纯化效果,尤其是对铁,条件是在欲精制的冶金级硅中铝和铁之间的重量比维持在某些限度内。同时发现,将要精炼的硅中低量的钙导致细颗粒硅的较低损失。
因此,本发明涉及一种纯化冶金级硅的方法,其中将含钙的化合物在硅从熔炉放出之前或之后加到熔融的硅中,然后铸造硅并固化,将固化的硅碾碎并经过由两个浸提步骤组成的纯化过程,在第一个浸提步骤中将硅用FeCl3或FeCl3和HCl的水溶液处理,这使得硅分解,而在第二个浸提步骤中用HF或HF/HNO3的水溶液对硅进行处理,该法的特征在于,加入到熔融硅中含钙化合物的量需要在熔融硅中提供0.3-0.95%重量的钙,而且在熔融硅中铝和铁的重量比通过加铝到熔融硅中调节到0.5-2.0。
铝和铁的重量比优选调节到0.6-1.2。
已令人惊异地发现,用本发明的方法可得到纯化硅中的铁含量与按照US No.4,539,194的方法处理的硅中的铁含量同样低,即使加到熔融硅中的钙量大大低于按照US No.4,539,194的方法。此外,对于发生在两个浸提步骤中的反应,得到了改进的控制,这是因为形成的硅烷的量大大减少,因而减低了爆炸的可能性。按照本发明的方法给出了改进的硅产率,因为已证实细颗粒形式的硅损失随钙含量的降低而减少。
发明的详细说明
实施例1
不同数量的钙和铝加到熔融的冶金级硅中。
合金在铸模中于较高冷却速率下浇铸。将固化的合金碾碎为颗粒尺寸低于120mm,而对某些合金而言颗粒尺寸小于30mm。这些合金的化学组成以及铝和铁的含量比示于表1。
表1中的2和3号合金是按照本发明的方法制成的,而表1中的1号和4号合金具有的铝和铁的重量比超出本发明的范围。
表1
元素 | Feppmw | Alppmw | Al/Fe | Cappmw | Tippmw | Pppmw | Bppmw |
合金1 | 2980 | 660 | 0.22 | 9200 | 140 | 39 | 7 |
合金2 | 2100 | 1300 | 0.62 | 8500 | 120 | 52 | 7 |
合金3 | 2410 | 1850 | 1.18 | 9200 | 180 | 38 | 7 |
合金4 | 2280 | 5860 | 2.57 | 10200 | 170 | 40 | 7 |
然后将合金用FeCl3和HCl的水溶液在第一浸提步骤中浸提。来自第一浸提步骤中未溶解的硅用水洗涤,然后用5%HF溶液进行第二浸提步骤。来自第二浸提步骤的固体硅用水洗涤。
分析纯化硅合金的杂质,结果示于表2。
表2
元素 | Feppmw | Alppmw | Cappmw | Tippmw | Pppmw | Bppmw |
合金1 | 82 | 52 | 450 | 10 | 24 | 6 |
合金2 | 50 | 70 | 310 | <10 | 16 | 8 |
合金3 | 55 | 162 | 441 | 7 | 20 | 6 |
合金4 | 75 | 210 | 255 | 11 | 20 | 6 |
由表2可看出,2号和3号合金的杂质去除大大好于1号和4号合金,1号和4号合金中Al/Fe重量比分别低于和高于2号和3号合金。
Claims (2)
1.纯化冶金级硅的方法,其中含钙化合物是在硅从熔炉放出之前或之后加到熔融硅中,然后铸造和固化硅,将固化的硅碾碎并经受由两个浸提步骤组成的纯化过程,在第一个浸提步骤中用FeCl3或FeCl3和HCl的水溶液处理硅,使硅分解,而在第二个浸提步骤中用HF或HF/HNO3的水溶液处理硅,其特征在于,加到熔融硅中的含钙化合物的量必须在熔融硅中提供0.3-0.95%重量的钙,和熔融硅中铝和铁的重量比通过把铝加到熔融硅中调节成0.5-2.0。
2.按照权利要求1的方法,其特征在于铝和铁的重量比控制在0.6-1.2。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NO19996022A NO313132B1 (no) | 1999-12-08 | 1999-12-08 | Fremgangsmåte for rensing av silisium |
NO19996022 | 1999-12-08 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1409691A CN1409691A (zh) | 2003-04-09 |
CN1231416C true CN1231416C (zh) | 2005-12-14 |
Family
ID=19904078
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB008169047A Expired - Lifetime CN1231416C (zh) | 1999-12-08 | 2000-11-08 | 冶金级硅的纯化方法 |
Country Status (12)
Country | Link |
---|---|
US (1) | US6861040B1 (zh) |
EP (1) | EP1254074B1 (zh) |
JP (1) | JP4035323B2 (zh) |
CN (1) | CN1231416C (zh) |
AT (1) | ATE277866T1 (zh) |
AU (1) | AU1560701A (zh) |
BR (1) | BR0016239B1 (zh) |
CA (1) | CA2393511C (zh) |
DE (1) | DE60014441T2 (zh) |
ES (1) | ES2223616T3 (zh) |
NO (1) | NO313132B1 (zh) |
WO (1) | WO2001042136A1 (zh) |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4115432B2 (ja) * | 2004-07-14 | 2008-07-09 | シャープ株式会社 | 金属の精製方法 |
CN100579902C (zh) * | 2007-07-06 | 2010-01-13 | 昆明理工大学 | 一种制备超冶金级硅的方法 |
ITMI20081085A1 (it) * | 2008-06-16 | 2009-12-17 | N E D Silicon S P A | Metodo per la preparazione di silicio di grado metallurgico di elevata purezza. |
CA2766721A1 (en) * | 2009-06-24 | 2010-12-29 | The Governing Council Of The University Of Toronto | Method of removal of impurities from silicon |
DE102009034317A1 (de) | 2009-07-23 | 2011-02-03 | Q-Cells Se | Verfahren zur Herstellung durchbruchsicherer p-Typ Solarzellen aus umg-Silizium |
NO331026B1 (no) | 2009-09-23 | 2011-09-12 | Elkem Solar As | Fremgangsmate for fremstilling av hoyrent silisium |
DE102009046265A1 (de) * | 2009-10-30 | 2011-05-19 | Rheinisch-Westfälische Technische Hochschule Aachen | Verfahren zur Aufarbeitung von Sägerückständen aus der Produktion von Silizium-Wafern |
WO2011146814A2 (en) | 2010-05-20 | 2011-11-24 | Dow Corning Corporation | Method and system for producing an aluminum-silicon alloy |
CN102602935B (zh) * | 2012-03-05 | 2014-03-12 | 矽明科技股份有限公司 | 一种高钙除磷的硅的清洗方法 |
KR101733325B1 (ko) | 2012-06-25 | 2017-05-08 | 실리코르 머티리얼즈 인코포레이티드 | 실리콘의 정제 방법 |
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 |
NO339608B1 (no) * | 2013-09-09 | 2017-01-09 | Elkem Solar As | Multikrystallinske silisiumingoter, silisiummasterlegering, fremgangsmåte for å øke utbyttet av multikrystallinske silisiumingoter for solceller |
WO2017096563A1 (zh) * | 2015-12-09 | 2017-06-15 | 季国平 | 一种硅的工业提纯方法 |
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US4200621A (en) * | 1978-07-18 | 1980-04-29 | Motorola, Inc. | Sequential purification and crystal growth |
IT1100218B (it) * | 1978-11-09 | 1985-09-28 | Montedison Spa | Procedimento per la purificazione di silicio |
US4312847A (en) * | 1979-05-24 | 1982-01-26 | Aluminum Company Of America | Silicon purification system |
DE2933164A1 (de) * | 1979-08-16 | 1981-02-26 | Consortium Elektrochem Ind | Verfahren zum reinigen von rohsilicium |
NO152551C (no) | 1983-02-07 | 1985-10-16 | Elkem As | Fremgangsmaate til fremstilling av rent silisium. |
US4612179A (en) * | 1985-03-13 | 1986-09-16 | Sri International | Process for purification of solid silicon |
US4798659A (en) * | 1986-12-22 | 1989-01-17 | Dow Corning Corporation | Addition of calcium compounds to the carbothermic reduction of silica |
RU2097320C1 (ru) | 1993-11-01 | 1997-11-27 | Институт металлургии Уральского отделения РАН | Способ получения порошка кремния повышенной частоты |
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- 1999-12-08 NO NO19996022A patent/NO313132B1/no not_active IP Right Cessation
-
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- 2000-08-11 US US10/149,176 patent/US6861040B1/en not_active Expired - Lifetime
- 2000-11-08 BR BRPI0016239-6A patent/BR0016239B1/pt not_active IP Right Cessation
- 2000-11-08 AU AU15607/01A patent/AU1560701A/en not_active Abandoned
- 2000-11-08 CN CNB008169047A patent/CN1231416C/zh not_active Expired - Lifetime
- 2000-11-08 DE DE60014441T patent/DE60014441T2/de not_active Expired - Lifetime
- 2000-11-08 EP EP00978115A patent/EP1254074B1/en not_active Expired - Lifetime
- 2000-11-08 CA CA002393511A patent/CA2393511C/en not_active Expired - Lifetime
- 2000-11-08 ES ES00978115T patent/ES2223616T3/es not_active Expired - Lifetime
- 2000-11-08 AT AT00978115T patent/ATE277866T1/de not_active IP Right Cessation
- 2000-11-08 JP JP2001543443A patent/JP4035323B2/ja not_active Expired - Fee Related
- 2000-11-08 WO PCT/NO2000/000374 patent/WO2001042136A1/en active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
NO996022L (no) | 2001-06-11 |
EP1254074A1 (en) | 2002-11-06 |
CA2393511A1 (en) | 2001-06-14 |
DE60014441T2 (de) | 2005-01-20 |
US6861040B1 (en) | 2005-03-01 |
EP1254074B1 (en) | 2004-09-29 |
JP2003516295A (ja) | 2003-05-13 |
ATE277866T1 (de) | 2004-10-15 |
BR0016239A (pt) | 2002-08-27 |
CN1409691A (zh) | 2003-04-09 |
NO996022D0 (no) | 1999-12-08 |
NO313132B1 (no) | 2002-08-19 |
AU1560701A (en) | 2001-06-18 |
ES2223616T3 (es) | 2005-03-01 |
DE60014441D1 (de) | 2004-11-04 |
BR0016239B1 (pt) | 2009-08-11 |
JP4035323B2 (ja) | 2008-01-23 |
CA2393511C (en) | 2007-03-20 |
WO2001042136A1 (en) | 2001-06-14 |
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