JP5190056B2 - 高純度で分級された多結晶性シリコン断片を製造するための方法および装置 - Google Patents
高純度で分級された多結晶性シリコン断片を製造するための方法および装置 Download PDFInfo
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- JP5190056B2 JP5190056B2 JP2009522203A JP2009522203A JP5190056B2 JP 5190056 B2 JP5190056 B2 JP 5190056B2 JP 2009522203 A JP2009522203 A JP 2009522203A JP 2009522203 A JP2009522203 A JP 2009522203A JP 5190056 B2 JP5190056 B2 JP 5190056B2
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims description 108
- 238000000034 method Methods 0.000 title claims description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 11
- 229920005591 polysilicon Polymers 0.000 claims description 104
- 238000004140 cleaning Methods 0.000 claims description 59
- 239000012634 fragment Substances 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 39
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 239000000956 alloy Substances 0.000 claims description 18
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 230000005693 optoelectronics Effects 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims 2
- 241001494479 Pecora Species 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000011109 contamination Methods 0.000 description 35
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 10
- 238000012545 processing Methods 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- AZUYLZMQTIKGSC-UHFFFAOYSA-N 1-[6-[4-(5-chloro-6-methyl-1H-indazol-4-yl)-5-methyl-3-(1-methylindazol-5-yl)pyrazol-1-yl]-2-azaspiro[3.3]heptan-2-yl]prop-2-en-1-one Chemical compound ClC=1C(=C2C=NNC2=CC=1C)C=1C(=NN(C=1C)C1CC2(CN(C2)C(C=C)=O)C1)C=1C=C2C=NN(C2=CC=1)C AZUYLZMQTIKGSC-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 229910001315 Tool steel Inorganic materials 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 241000255777 Lepidoptera Species 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Images
Classifications
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- 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
- C30B29/06—Silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C21/00—Disintegrating plant with or without drying of the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
-
- 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
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C2210/00—Codes relating to different types of disintegrating devices
- B02C2210/02—Features for generally used wear parts on beaters, knives, rollers, anvils, linings and the like
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Food Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Disintegrating Or Milling (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
数多くのバッチ量でポリシリコン断片の金属表面値に対する種々の加工工具の影響または種々の汚染する材料の影響を試験した。
1.前清浄化:25+/−5℃で水と共にHF5質量%、HCl8質量%およびH2O23質量%を含有するHF/HCl/H2O2水溶液で20分間の酸洗。シリコンの腐蝕による剥削は、約0.02μmであった。
2.22℃で5分間の洗浄。
3.主要な清浄化:水と共にHF3質量%およびHNO365質量%を含有するHF/HNO3水溶液中での8℃で5分間の腐蝕。腐蝕による剥削は、約12μmであった。
4.22℃で5分間の洗浄。
5.22℃で水と共にHCl8質量%およびH2O22質量%を含有するHF/HCl/H2O2水溶液で5分間の親水性化。
6.22℃での洗浄。
7.80℃で等級100の最も純粋な空気での乾燥。
例1aの記載と同様に、汚染の少ない材料の公知技術水準から公知の使用は、清浄化後に表面に僅かな金属汚染を有するポリシリコン断片を提供する。都合の悪いことに、この材料は、全ての装置部材(例えば、針状部を備えた破砕用シャーレ)には、技術的に使用不可能である。製造可能である場合には、この種の装置部材は、極めて高価であり、ひいては非経済的である。その上、硬質金属(炭化タングステン)は、第1表中の例1aのための若干高められたタングステン値に明らかであるように処理によって劣悪に溶解される。
ジーメンス反応器からのポリシリコンロッドを図1に記載の装置によりポリシリコン断片に細断し、種々の大きさに選別し、この場合には、製品中に汚染する全ての装置部材は、例1bの記載と同様に低合金鋼から形成されている。
1.前清浄化:25+/−5℃で水と共にHF5質量%、HCl8質量%およびH2O23質量%を含有するHF/HCl/H2O2水溶液で20分間の酸洗。シリコンの腐蝕による剥削は、約0.02μmであった。
2.22℃での5分間の洗浄。
3.主要な清浄化:水と共にHF3質量%およびHNO365質量%を含有するHF/HNO3水溶液中で8℃で5分間の腐蝕。腐蝕による剥削は、約12μmであった。
4.5分間の洗浄。
5.22℃で水と共にHCl8質量%およびH2O22質量%を含有するHF/HCl/H2O2水溶液で5分間の親水性化。
6.22℃での洗浄。
7.80℃で等級100の最も純粋な空気での乾燥。
Claims (9)
- ジーメンス法からのポリシリコンを、細断工具およびスクリーン装置を含む装置により細断し、分級し、こうして得られたポリシリコン断片を清浄化浴により清浄化することにより、高純度の分級されたポリシリコン断片を製造する方法において、細断工具およびスクリーン装置が、5質量%未満の合金含量を有する低合金鋼の材料からなる、ポリシリコンと接触する表面を例外なく有し、清浄化浴が、化合物の弗化水素酸、塩酸および過酸化水素を含有する酸化性清浄化溶液での少なくとも1つの段階での前清浄化、硝酸および弗化水素酸を含有する清浄化溶液での他の段階での主要清浄化、および酸化性清浄化溶液での他の段階によるポリシリコン断片の親水性化を含むことを特徴とする、高純度の分級されたポリシリコン断片を製造する方法。
- ポリシリコンと接触する、ポリシリコンの破砕、搬送/輸送、および分級に使用される全ての部分的装置の表面が例外なく5質量%未満の合金含量を有する低合金鋼の材料から形成され、この材料が分級されたポリシリコン断片の次の清浄化で簡単に完全に、分級されたポリシリコン断片から除去される、請求項1記載の方法。
- ポリシリコンの破砕、分級および清浄化のための部分的装置を含む請求項1記載の方法を実施するための装置であって、ポリシリコンの破砕および分級に使用される全ての部分的装置の表面が例外なく5質量%未満の合金含量を有する低合金鋼の材料から形成されている装置。
- さらに、ポリシリコンの搬送のための部分的装置を含み、ポリシリコンの搬送に使用される部分的装置の表面が5質量%未満の合金含量を有する低合金鋼の材料から形成されている請求項3記載の装置。
- 前記装置が、破砕装置中への粗大なポリシリコン断片の供給装置、この破砕装置、この破砕装置から選別装置への搬送装置およびポリシリコン断片を分級するための選別装置を含む、請求項3または4記載の装置。
- 破砕装置が、ロール型破砕機またはジョークラッシャーを含む、請求項5記載の装置。
- 破砕装置が、シープスフートローラを含む、請求項5記載の装置。
- 選別装置が、多段階の機械的スクリーン装置と多段階の光電子式分離装置とからなる、請求項5から7までのいずれか1項に記載の装置。
- さらに、前記装置が前細断機を含む、請求項3から7までのいずれか1項に記載の装置。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006035081A DE102006035081A1 (de) | 2006-07-28 | 2006-07-28 | Verfahren und Vorrichtung zur Herstellung von klassiertem polykristallinen Siliciumbruch in hoher Reinheit |
DE102006035081.2 | 2006-07-28 | ||
PCT/EP2007/057238 WO2008012215A1 (de) | 2006-07-28 | 2007-07-13 | Verfahren und vorrichtung zur herstellung von klassiertem polykristallinen siliciumbruch in hoher reinheit |
Publications (3)
Publication Number | Publication Date |
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JP2009544564A JP2009544564A (ja) | 2009-12-17 |
JP2009544564A5 JP2009544564A5 (ja) | 2012-06-21 |
JP5190056B2 true JP5190056B2 (ja) | 2013-04-24 |
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Application Number | Title | Priority Date | Filing Date |
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JP2009522203A Active JP5190056B2 (ja) | 2006-07-28 | 2007-07-13 | 高純度で分級された多結晶性シリコン断片を製造するための方法および装置 |
Country Status (8)
Country | Link |
---|---|
US (1) | US9340901B2 (ja) |
EP (1) | EP2047014B1 (ja) |
JP (1) | JP5190056B2 (ja) |
KR (1) | KR101180177B1 (ja) |
CN (1) | CN101495682B (ja) |
CA (1) | CA2657007C (ja) |
DE (1) | DE102006035081A1 (ja) |
WO (1) | WO2008012215A1 (ja) |
Families Citing this family (38)
Publication number | Priority date | Publication date | Assignee | Title |
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DE102007027110A1 (de) * | 2007-06-13 | 2008-12-18 | Wacker Chemie Ag | Verfahren und Vorrichtung zum Verpacken von polykristallinem Siliciumbruch |
DE102007031471A1 (de) * | 2007-07-05 | 2009-01-08 | Schott Solar Gmbh | Verfahren zur Aufbereitung von Siliciummaterial |
CN101624724B (zh) * | 2008-08-22 | 2012-07-25 | 江西赛维Ldk光伏硅科技有限公司 | 多根多晶硅棒的取棒方法及其取棒装置和取棒装置组合件 |
CA2766721A1 (en) * | 2009-06-24 | 2010-12-29 | The Governing Council Of The University Of Toronto | Method of removal of impurities from silicon |
DE102010039752A1 (de) * | 2010-08-25 | 2012-03-01 | Wacker Chemie Ag | Polykristallines Silicium und Verfahren zu dessen Herstellung |
DE102010040836A1 (de) | 2010-09-15 | 2012-03-15 | Wacker Chemie Ag | Verfahren zur Herstellung von Silicium-Dünnstäben |
CN102059170B (zh) * | 2010-11-26 | 2011-10-19 | 镇江荣德新能源科技有限公司 | 一种破碎多晶硅棒的装置及方法 |
DE102011003875A1 (de) * | 2011-02-09 | 2012-08-09 | Wacker Chemie Ag | Verfahren und Vorrichtung zum Dosieren und Verpacken von Polysiliciumbruchstücken sowie Dosier- und Verpackungseinheit |
US8906453B2 (en) * | 2011-03-18 | 2014-12-09 | MEMC Electronics Materials, S.p.A. | Tool for harvesting polycrystalline silicon-coated rods from a chemical vapor deposition reactor |
DE102011089449A1 (de) | 2011-12-21 | 2013-06-27 | Wacker Chemie Ag | Polykristalliner Siliciumstab und Verfahren zur Herstellung von Polysilicium |
DE102011089356A1 (de) | 2011-12-21 | 2013-06-27 | Wacker Chemie Ag | Polykristallines Siliciumstück und Verfahren zum Brechen eines Siliciumkörpers |
DE102012200992A1 (de) | 2012-01-24 | 2013-07-25 | Wacker Chemie Ag | Dotierstoffarmes polykristallines Siliciumstück |
DE102012200994A1 (de) * | 2012-01-24 | 2013-07-25 | Wacker Chemie Ag | Verfahren zur Bestimmung einer Oberflächen-Verunreinigung von polykristallinem Silicium |
US9749136B2 (en) * | 2012-02-24 | 2017-08-29 | Comcast Cable Communications, Llc | Method for watermarking content |
DE102012208473A1 (de) | 2012-05-21 | 2013-11-21 | Wacker Chemie Ag | Polykristallines Silicium |
DE102012213869A1 (de) * | 2012-08-06 | 2014-02-06 | Wacker Chemie Ag | Polykristalline Siliciumbruchstücke und Verfahren zu deren Herstellung |
DE102012220422A1 (de) | 2012-11-09 | 2014-05-15 | Wacker Chemie Ag | Verpackung von polykristallinem Silicium |
DE102013206339A1 (de) | 2013-04-10 | 2014-10-16 | Wacker Chemie Ag | Vorrichtung und Verfahren zum Ausbau von polykristallinen Siliciumstäben aus einem Reaktor |
DE102013206436A1 (de) | 2013-04-11 | 2014-10-16 | Wacker Chemie Ag | Reinigung von CVD-Produktionsräumen |
DE102013215257A1 (de) * | 2013-08-02 | 2015-02-05 | Wacker Chemie Ag | Verfahren zum Zerkleinern von Silicium und Verwendung des zerkleinerten Siliciums in einer Lithium-Ionen-Batterie |
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DE102013223883A1 (de) * | 2013-11-22 | 2015-05-28 | Wacker Chemie Ag | Verfahren zur Herstellung von polykristallinem Silicium |
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CN101495682A (zh) | 2009-07-29 |
KR101180177B1 (ko) | 2012-09-05 |
EP2047014B1 (de) | 2013-12-25 |
KR20090054426A (ko) | 2009-05-29 |
JP2009544564A (ja) | 2009-12-17 |
DE102006035081A1 (de) | 2008-01-31 |
EP2047014A1 (de) | 2009-04-15 |
WO2008012215A1 (de) | 2008-01-31 |
US9340901B2 (en) | 2016-05-17 |
CA2657007A1 (en) | 2008-01-31 |
CN101495682B (zh) | 2013-03-13 |
CA2657007C (en) | 2011-09-13 |
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