WO2011111335A1 - トリクロロシランの製造方法 - Google Patents
トリクロロシランの製造方法 Download PDFInfo
- Publication number
- WO2011111335A1 WO2011111335A1 PCT/JP2011/001189 JP2011001189W WO2011111335A1 WO 2011111335 A1 WO2011111335 A1 WO 2011111335A1 JP 2011001189 W JP2011001189 W JP 2011001189W WO 2011111335 A1 WO2011111335 A1 WO 2011111335A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- trichlorosilane
- methyldichlorosilane
- tetrachlorosilane
- chlorine
- redistribution
- Prior art date
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Classifications
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- 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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- 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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
-
- 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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
- C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from 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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
Definitions
- the present invention relates to a method for producing trichlorosilane, and more particularly to a method for facilitating separation of trichlorosilane and methyldichlorosilane to obtain high-purity trichlorosilane.
- Trichlorosilane (HSiCl 3 ) has long been used as a raw material for high-purity polycrystalline silicon used in the production of silicon wafers and the like. Many synthetic methods are known as methods for obtaining trichlorosilane, and Japanese Patent Application Laid-Open No. 56-73617 (Patent Document 1) discloses that by-product silicon tetrachloride is efficiently used in the production of trichlorosilane. An invention of a method for producing trichlorosilane, characterized by being converted to trichlorosilane, is disclosed.
- Patent Document 2 Japanese Patent Laid-Open No. 9-169514.
- Gazette (see Patent Document 3) and the like), a method in which silicon tetrachloride is reacted with hydrogen in the presence of metallurgical grade silicon to reduce it to trichlorosilane (see JP-A-60-36318 (Patent Document 4)), the above Known is a method in which copper tetrachloride is used in place of metallurgical grade silicon and silicon tetrachloride is reacted with hydrogen in the presence of copper silicide to reduce it to trichlorosilane (see JP-A-10-29813 (Patent Document 5)). It has been.
- Carbon impurities in silicon crystals form impurity levels in the band gap and act as traps for carriers, or accelerate the formation of oxygen precipitation nuclei in the crystal and cause defects during the semiconductor device manufacturing process. Therefore, the content of carbon impurities is also a problem in semiconductor grade polycrystalline silicon.
- low boiling point methylchlorosilanes as by-products derived from carbon impurities are several tens of weights. About ppm is mixed.
- methyldichlorosilane has its boiling point (41 ° C.) close to the boiling point (32 ° C.) of trichlorosilane which is the subject of distillation purification. It is difficult.
- Patent Document 7 discloses a method for purifying trichlorosilane capable of reducing the carbon impurity concentration at a relatively low cost.
- a technique is adopted in which the carbon-containing silicon chloride compound in trichlorosilane is uniformly removed regardless of the boiling point by contacting with an adsorbent such as silica gel or activated carbon.
- the present invention has been made in view of such problems, and the object of the present invention is to eliminate the conventional method when producing high-purity trichlorosilane without requiring an excessive distillation purification step. It is an object of the present invention to provide a method for facilitating removal of methyldichlorosilane, which has been difficult to achieve.
- the method for producing trichlorosilane of the present invention comprises a high-purity trichlorosilane (CH 3 HSiCl 2 ), a tetrachlorosilane (SiCl 4 ), and a trichlorosilane (HSiCl 3 ).
- a method for obtaining chlorosilane comprising the following steps.
- the redistribution of chlorine in the step (B) is performed in a temperature range of 300 to 600 ° C.
- the chlorine redistribution in the step (B) can be performed without using a catalyst.
- the redistribution of chlorine in the step (B) may be performed in a hydrogen-containing reducing atmosphere in a heating vessel using silicon containing copper chloride as a catalyst as a fluidized bed. .
- the mixture containing methyldichlorosilane, tetrachlorosilane, and trichlorosilane is, for example, a product obtained by synthesizing trichlorosilane by a reaction between metallurgical grade silicon and hydrogen chloride, trichlorosilane from trichlorosilane in a hydrogen-containing reducing atmosphere.
- These include products in the conversion reaction to chlorosilane, reaction products discharged in the polycrystalline silicon manufacturing process using trichlorosilane as a raw material, and the like.
- methyldichlorosilane (boiling point 41 ° C.), which has been difficult to remove because the boiling point is close to the boiling point (32 ° C.) of trichlorosilane that is the subject of distillation purification, is converted with tetrachlorosilane. Removal is facilitated by conversion to methyltrichlorosilane (boiling point 66 ° C.) by redistributing chlorine between them.
- methyldichlorosilane in trichlorosilane which is difficult to be separated by distillation, is converted to a compound having a higher boiling point, so that the purification load of high-purity trichlorosilane by distillation can be reduced. It becomes.
- FIGS. 1 to 3 are examples of flow charts of the method for producing trichlorosilane according to the present invention.
- methyldichlorosilane (CH 3 HSiCl 2 ), tetrachlorosilane (SiCl 4 ) and trichlorosilane ( HSiCl 3 ) is distilled to fractionate a fraction having a higher methyldichlorosilane content than the mixture before distillation (S101), and the fractionated fraction is heated to obtain methyldichlorosilane and tetrachlorosilane. And redistributing chlorine to convert methyldichlorosilane into methyltrichlorosilane (CH 3 SiCl 3 ) (S102).
- methyldichlorosilane (boiling point 41 ° C.), which has been difficult to remove because its boiling point is close to the boiling point (32 ° C.) of trichlorosilane, which is the object of distillation purification, is redistributed with tetrachlorosilane. This makes it easy to remove by converting to methyltrichlorosilane (boiling point 66 ° C.).
- methyldichlorosilane in trichlorosilane which is difficult to be separated by distillation, is converted to a compound having a higher boiling point, so that the purification load of high-purity trichlorosilane by distillation can be reduced. It becomes.
- Trichlorosilane or the like can be used as the chlorine donor for the above-mentioned chlorine redistribution, but it is considered that tetrachlorosilane is converted to trichlorosilane by chlorine donation in the present invention. This is because it is always present in the mixture produced by the trichlorosilane synthesis reaction, and it is not necessary to add a new one from the outside.
- tetrachlorosilane is a product (S100A) for synthesizing trichlorosilane by the reaction of metallurgical grade silicon and hydrogen chloride, or during the conversion reaction from tetrachlorosilane to trichlorosilane in a hydrogen-containing reducing atmosphere. Since it is always contained in the product (S100B) or the reaction product (S100C) discharged in the polycrystalline silicon manufacturing process using trichlorosilane as a raw material, chlorine should be used. There is no need to add a donor from the outside, and there is an advantage that after chlorine donation, it is converted to trichlorosilane which is an object of distillation purification and the yield is also increased.
- the main product is trichlorosilane.
- trichlorosilane and tetrachlorosilane are obtained in a ratio of approximately 80:20 to 20:80.
- the above-mentioned chlorine redistribution reaction can also be carried out without using a special catalyst. In this case, there is an advantage that there is no fear of carbon impurities being mixed in the chlorine redistribution reaction step. It may be carried out in a hydrogen-containing reducing atmosphere in a heating vessel using silicon contained as a fluidized bed.
- the chlorine redistribution reaction is preferably performed at 300 ° C. or higher, more preferably 400 ° C. or higher because the redistribution rate increases as the temperature increases.
- the chlorine redistribution reaction system contains hydrogen at a temperature of 900 ° C. or higher, there is a possibility that the reduction reaction by the hydrogen and the redistribution reaction of chlorine from tetrachlorosilane compete. For this reason, it is preferable that the upper limit of temperature shall be 600 degreeC.
- the pressure at the time of performing the chlorine redistribution reaction can be, for example, in the range of 0.1 to 4.0 MPa, but it is preferable to perform the pressure as high as possible from the viewpoint of improving productivity. On the other hand, if the reaction is carried out under a pressure exceeding 4.0 MPa, a liquefaction phenomenon may occur in the reaction vessel, which is not preferable from the viewpoint of ensuring safety.
- the reaction time depends on the presence or absence of the catalyst, the reaction temperature and the pressure, but a constant reaction rate can be obtained if it is 10 to 30 seconds or longer. From the viewpoint of productivity of trichlorosilane, it is preferably set within a range of 30 to 200 seconds.
- the crude product when such a chlorine redistribution reaction is incorporated into the production process of trichlorosilane by the direct method or the production process of trichlorosilane by reduction of tetrachlorosilane, the crude product contains a relatively large amount of tetrachlorosilane. Therefore, the crude product may be subjected to chlorine redistribution treatment as it is.
- the content of tetrachlorosilane in the crude product is low, or when trichlorosilane containing a large amount (several tens to several hundred ppm) of methyldichlorosilane collected by distillation is recovered, it is externally applied. It is also possible to introduce tetrachlorosilane as a chlorine donor separately.
- a carrier gas such as hydrogen or an inert gas should be used. Also good.
- hydrogen when using hydrogen as carrier gas, you may recycle and use the hydrogen used in the manufacturing process of the trichlorosilane by the direct method, and the manufacturing process of the trichlorosilane by the reduction
- Example 1 Chlorine redistribution effect: Using a hollow reactor (reactor A) and a reactor (reactor B) with a fluidized bed of metallurgical grade metal silicon, the methylchlorosilanes in the mixture of chlorosilanes The redistribution effect was verified. A stainless steel tube having a diameter of 40 cm and a length of 100 cm was used as the reactor.
- silicon tetrachloride containing 180 ppmwt of methyldichlorosilane was diluted with a 2-fold molar amount of hydrogen and introduced in a gas state.
- the reactor was heated to 500 ° C. and supplied so that the evaluation target gas cylinder linear velocity was 1.0 cm / sec.
- the residence time with respect to the soaking range was about 50 seconds.
- the reactor internal pressure was maintained at 2.0 MPa.
- Example 2 Effect of using copper chloride (CuCl) as a catalyst: Metallurgical grade metal silicon containing 4 wt% of copper chloride (CuCl) as a catalyst, which was made into a stainless steel tube reactor (inner diameter 4 cm, long 100 cm) was filled to a height of 50 cm, and silicon tetrachloride containing 180 ppmwt of methyldichlorosilane was supplied to the reactor together with a double molar amount of hydrogen.
- the chlorine redistribution reaction conditions are a pressure of 2.0 MPa, a temperature of 500 ° C., and a residence time of 100 seconds.
- the ratio of trichlorosilane (TCS) to tetrachlorosilane (STC) (TCS / STC) in the finally obtained chlorosilane mixed product is approximately 3/7, methyldichlorosilane is reduced to 7.9 ppmwt, 150 ppmwt of chlorosilane was produced.
- methyldichlorosilane in trichlorosilane which is difficult to separate by distillation, is converted to a compound having a higher boiling point, so that the purification load of high-purity trichlorosilane by distillation can be reduced. It becomes. That is, according to the present invention, a method for obtaining a high purity trichlorosilane by facilitating the separation of trichlorosilane and methyldichlorosilane is provided.
- S100A, S100B, S100C Step of producing a mixture containing methyldichlorosilane, tetrachlorosilane and trichlorosilane
- S101 Distilling a mixture containing methyldichlorosilane, tetrachlorosilane and trichlorosilane to obtain methyl Step of fractionating a fraction having a high chlorosilane content
- S102 Step of converting methyldichlorosilane to methyltrichlorosilane by chlorine redistribution
- S103 Distilling and purifying the fraction after redistribution containing methyltrichlorosilane to high purity Step of separating trichlorosilane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
Description
CH3SiHCl2 + HCl → SiHCl3 + CH4
CH3SiHCl2 + SiCl4 → CH3SiCl3 + SiHCl3
CH3SiHCl2 + SiHCl3 → CH3SiCl3 + SiH2Cl2
CH3SiHCl2 + H2 → SiH2Cl2 + CH4
CH3SiCl3 + H2 → SiHCl3 + CH4
S101:メチルジクロロシランとテトラクロロシランとトリクロロシランとを含む混合物を蒸留して蒸留前混合物よりもメチルジクロロシラン含有率が高い留分を分画する工程
S102:塩素再配分によりメチルジクロロシランをメチルトリクロロシランに変換する工程
S103:メチルトリクロロシランを含む再分配後の留分を蒸留精製して高純度なトリクロロシランを分離する工程
Claims (7)
- メチルジクロロシラン(CH3HSiCl2)とテトラクロロシラン(SiCl4)とトリクロロシラン(HSiCl3)とを含む混合物から高純度のトリクロロシランを得る方法であって、下記の工程を備えているトリクロロシランの製造方法。
(A)前記混合物を蒸留して蒸留前混合物よりもメチルジクロロシラン含有率が高い留分を分画する工程:
(B)前記分画された留分を加熱してメチルジクロロシランとテトラクロロシランとの間で塩素の再分配を行って前記メチルジクロロシランをメチルトリクロロシラン(CH3SiCl3)に変換する工程:
(C)前記メチルトリクロロシラン(CH3SiCl3)を含む再分配後の留分を蒸留精製してトリクロロシランを分離する工程。 - 前記工程(B)における塩素の再分配を、300~600℃の温度範囲で行う請求項1に記載のトリクロロシランの製造方法。
- 前記工程(B)における塩素の再分配を、触媒を用いずに実行する請求項2に記載のトリクロロシランの製造方法。
- 前記工程(B)における塩素の再分配を、塩化銅を触媒として含有させたシリコンを流動床とする加熱容器内において水素含有還元性雰囲気下で実行する請求項2に記載のトリクロロシランの製造方法。
- 前記メチルジクロロシランとテトラクロロシランとトリクロロシランとを含む混合物は、冶金級シリコンと塩化水素との反応によりトリクロロシランを合成する際の生成物である請求項1乃至4の何れか1項に記載のトリクロロシランの製造方法。
- 前記メチルジクロロシランとテトラクロロシランとトリクロロシランとを含む混合物は、水素含有還元性雰囲気下でのテトラクロロシランからトリクロロシランへの転換反応の際の生成物である請求項1乃至4の何れか1項に記載のトリクロロシランの製造方法。
- 前記メチルジクロロシランとテトラクロロシランとトリクロロシランとを含む混合物は、トリクロロシランを原料とする多結晶シリコン製造工程で排出される反応生成物である請求項1乃至4の何れか1項に記載のトリクロロシランの製造方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201180013151.5A CN102791630B (zh) | 2010-03-10 | 2011-03-01 | 三氯硅烷的制造方法 |
AU2011225614A AU2011225614B2 (en) | 2010-03-10 | 2011-03-01 | Method for producing trichlorosilane |
US13/583,794 US9266742B2 (en) | 2010-03-10 | 2011-03-01 | Method for producing trichlorosilane |
EP11753001.4A EP2546197B1 (en) | 2010-03-10 | 2011-03-01 | Method for producing trichlorosilane |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2010-052548 | 2010-03-10 | ||
JP2010052548A JP5337749B2 (ja) | 2010-03-10 | 2010-03-10 | トリクロロシランの製造方法 |
Publications (1)
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WO2011111335A1 true WO2011111335A1 (ja) | 2011-09-15 |
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Application Number | Title | Priority Date | Filing Date |
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PCT/JP2011/001189 WO2011111335A1 (ja) | 2010-03-10 | 2011-03-01 | トリクロロシランの製造方法 |
Country Status (6)
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US (1) | US9266742B2 (ja) |
EP (1) | EP2546197B1 (ja) |
JP (1) | JP5337749B2 (ja) |
CN (1) | CN102791630B (ja) |
AU (1) | AU2011225614B2 (ja) |
WO (1) | WO2011111335A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108892143A (zh) * | 2018-09-28 | 2018-11-27 | 洛阳中硅高科技有限公司 | 提纯三氯氢硅的方法 |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5909153B2 (ja) | 2012-06-14 | 2016-04-26 | 信越化学工業株式会社 | 高純度多結晶シリコンの製造方法 |
CN103112858B (zh) * | 2013-01-15 | 2015-02-25 | 宁波大学 | 多晶硅副产物中二氯二氢硅的液相氯化方法 |
JP5879283B2 (ja) * | 2013-02-13 | 2016-03-08 | 信越化学工業株式会社 | トリクロロシランの製造方法 |
DE102015210762A1 (de) | 2015-06-12 | 2016-12-15 | Wacker Chemie Ag | Verfahren zur Aufarbeitung von mit Kohlenstoffverbindungen verunreinigten Chlorsilanen oder Chlorsilangemischen |
JP6586405B2 (ja) * | 2016-09-28 | 2019-10-02 | 信越化学工業株式会社 | トリクロロシランの精製システムおよび多結晶シリコンの製造方法 |
US10584035B2 (en) * | 2017-02-24 | 2020-03-10 | Shin-Etsu Chemical Co., Ltd. | Purification system of trichlorosilane and silicon crystal |
WO2019154502A1 (de) * | 2018-02-08 | 2019-08-15 | Wacker Chemie Ag | Verfahren zur klassifizierung von metallurgischem silicium |
EP3620436A1 (en) * | 2018-09-10 | 2020-03-11 | Momentive Performance Materials Inc. | Synthesis of trichlorosilane from tetrachlorosilane and hydridosilanes |
CN108946742A (zh) * | 2018-09-28 | 2018-12-07 | 洛阳中硅高科技有限公司 | 提纯三氯氢硅的装置 |
CN109179426A (zh) * | 2018-11-19 | 2019-01-11 | 天津科技大学 | 一种反应精馏去除三氯氢硅中甲基二氯硅烷的装置和方法 |
CN114956092A (zh) * | 2022-04-21 | 2022-08-30 | 新疆大全新能源股份有限公司 | 一种分离三氯氢硅中一甲基二氯硅烷杂质的方法 |
CN115650242A (zh) * | 2022-11-21 | 2023-01-31 | 青海黄河上游水电开发有限责任公司新能源分公司 | 三氯氢硅除碳装置及三氯氢硅除碳方法 |
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2010
- 2010-03-10 JP JP2010052548A patent/JP5337749B2/ja active Active
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2011
- 2011-03-01 AU AU2011225614A patent/AU2011225614B2/en not_active Ceased
- 2011-03-01 WO PCT/JP2011/001189 patent/WO2011111335A1/ja active Application Filing
- 2011-03-01 CN CN201180013151.5A patent/CN102791630B/zh active Active
- 2011-03-01 US US13/583,794 patent/US9266742B2/en active Active
- 2011-03-01 EP EP11753001.4A patent/EP2546197B1/en active Active
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CN108892143A (zh) * | 2018-09-28 | 2018-11-27 | 洛阳中硅高科技有限公司 | 提纯三氯氢硅的方法 |
Also Published As
Publication number | Publication date |
---|---|
US9266742B2 (en) | 2016-02-23 |
EP2546197A1 (en) | 2013-01-16 |
AU2011225614A1 (en) | 2012-10-11 |
US20130001063A1 (en) | 2013-01-03 |
CN102791630A (zh) | 2012-11-21 |
CN102791630B (zh) | 2014-11-19 |
JP5337749B2 (ja) | 2013-11-06 |
EP2546197B1 (en) | 2016-08-24 |
JP2011184255A (ja) | 2011-09-22 |
AU2011225614B2 (en) | 2013-03-28 |
EP2546197A4 (en) | 2015-05-06 |
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