JP4474409B2 - カーボンナノチューブの製造方法および製造装置 - Google Patents
カーボンナノチューブの製造方法および製造装置 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 35
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 43
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 42
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 42
- 239000011261 inert gas Substances 0.000 claims abstract description 30
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 27
- 239000012298 atmosphere Substances 0.000 claims abstract description 22
- 239000011949 solid catalyst Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 12
- 239000005977 Ethylene Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 239000002071 nanotube Substances 0.000 abstract description 8
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 25
- 230000015572 biosynthetic process Effects 0.000 description 22
- 238000003786 synthesis reaction Methods 0.000 description 21
- 229910052799 carbon Inorganic materials 0.000 description 19
- 239000000047 product Substances 0.000 description 17
- 239000012159 carrier gas Substances 0.000 description 13
- 238000005229 chemical vapour deposition Methods 0.000 description 13
- 238000011084 recovery Methods 0.000 description 11
- 238000011144 upstream manufacturing Methods 0.000 description 11
- 238000009826 distribution Methods 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000012080 ambient air Substances 0.000 description 5
- 239000012495 reaction gas Substances 0.000 description 5
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- 230000009849 deactivation Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
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- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 229930195734 saturated hydrocarbon Natural products 0.000 description 3
- 239000002109 single walled nanotube Substances 0.000 description 3
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 239000003779 heat-resistant material Substances 0.000 description 2
- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 230000002028 premature Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000001628 carbon nanotube synthesis method Methods 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
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- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
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- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
- B01J8/003—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor in a downward flow
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Description
・装置を不活性雰囲気下におくこと、
・新しい触媒を含む受け器を挿入するために反応炉を開けること、
・装置を不活性雰囲気下におくこと、
・不活性ガス中で反応炉に炭化水素を供給すること、
・装置を不活性雰囲気下におくこと、
・触媒を有する受け器および生の合成生成物を反応炉から回収すること。
以下に説明する実施例1ないし実施例3では、図1ないし図4に示す装置と同様な装置中で本発明による方法に従って実施したカーボンナノチューブの合成に関する試みを扱う。
触媒床の厚さ:0.22g/cm
反応炉の回転速度:2回転/分
キャリアガス中のエチレンのモル滴定濃度:0.50
触媒の分配速度:0.015g/秒
ガスの分配速度:3Nl/分
生産量:48g/時間
収率:触媒1gあたり4.9gのカーボン
触媒床の厚さ:0.04g/cm
反応炉の回転速度:2回転/分
キャリアガス中のエチレンのモル滴定濃度:0.33
触媒の分配速度:0.003g/秒
ガスの分配速度:3Nl/分
生産量:32g/時間
収率:触媒1gあたり3.8gのカーボン
以下に説明する実施例4ないし実施例6では、CCVD法の既知の不連続なモードに従って実施した。これらの例では、実施例1ないし実施例3の第1のシリーズで使用したのと同じ触媒を使用した。
永久触媒床の長さ:20cm
永久触媒床の質量:0.8g
キャリアガス中のエチレンのモル滴定濃度:0.33
ガスの分配速度:3Nl/分
不連続な試みの持続時間:20分
生産量:3.4g/時間
収率:触媒1gあたり2.1gのカーボン
永久触媒床の長さ:20cm
永久触媒床の質量:1.6g
キャリアガス中のエチレンのモル滴定濃度:0.33
ガスの分配速度:3Nl/分
不連続な試みの持続時間:20分
生産量:7.4g/時間
収率:触媒1gあたり2.3gのカーボン
Claims (9)
- 反応炉中での固体触媒の存在下における少なくとも1つの気体炭化水素の熱分解によるカーボンナノチューブの製造方法であって、前記反応炉の、前記炭化水素の分解が引き起こされる最適温度を生じる領域に、前記炭化水素および前記触媒を別個にかつ連続的に導入し、不活性雰囲気下で維持されたインレットロックチャンバを介して前記反応炉内に前記触媒を導入し、かつ、不活性ガスの流れで洗浄されるアウトレットロックチャンバを介して前記カーボンナノチューブを前記反応炉から回収することを特徴とするカーボンナノチューブの製造方法。
- 前記インレットロックチャンバと前記アウトレットロックチャンバの間で水平方向に対して傾斜して配設される管状反応炉を用い、前記管状反応炉を連続的に回転させることを特徴とする、請求項1に記載のカーボンナノチューブの製造方法。
- 前記温度を500〜1200℃の範囲から選択することを特徴とする、請求項1または2に記載のカーボンナノチューブの製造方法。
- 前記インレットチャンバ及び前記アウトレットチャンバから隔離して前記反応炉を加熱することを特徴とする、請求項1ないし3のうちのいずれか一項に記載のカーボンナノチューブの製造方法。
- さらに水素および/または不活性ガスを前記反応炉内に導入することを特徴とする、請求項1ないし4のうちのいずれか一項に記載のカーボンナノチューブの製造方法。
- アルゴン、窒素、およびヘリウムのうちから前記不活性ガスを選択することを特徴とする、請求項1ないし5のうちのいずれか一項に記載のカーボンナノチューブの製造方法。
- メタン、エチレン、およびアセチレンのうちから前記炭化水素を選択することを特徴とする、請求項1ないし6のうちのいずれか一項に記載のカーボンナノチューブの製造方法。
- 水平方向に対して傾斜した管状反応炉(4)と、気体試薬を前記反応炉に入れるためのデバイス(14)と、前記反応炉の同じ側の互いの近傍に開口する、粉状製品を装填するためのデバイス(16、17、21)と、前記反応炉から粉末を回収するためのデバイス(35、36、39、40)と、前記反応炉を加熱するためのデバイス(6)とを備え、前記装填デバイスは、2つのバルブ(18、19)によって隔離されたロックチャンバ(17)を備え、かつ、不活性ガス循環路への接続部(22、23)が設けられ、前記回収デバイスは、2つのバルブ(36、38)によって隔離された別のロックチャンバ(37)を備え、かつ、不活性ガス循環路への接続部(39、40)が設けられていることを特徴とする、請求項1ないし7のうちのいずれか一項に記載の方法を用いるカーボンナノチューブ製造装置。
- 前記装填デバイス(16、17、20、21、34)は、前記粉状製品の分配器(21)を備えることを特徴とする、請求項8に記載のカーボンナノチューブ製造装置。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03075349A EP1445236A1 (fr) | 2003-02-05 | 2003-02-05 | Procédé et installation pour la fabrication de nanotubes de carbone |
PCT/EP2004/000952 WO2004069742A1 (fr) | 2003-02-05 | 2004-01-28 | Procede et installation pour la fabrication de nanotubes de carbone |
Publications (2)
Publication Number | Publication Date |
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JP2006516946A JP2006516946A (ja) | 2006-07-13 |
JP4474409B2 true JP4474409B2 (ja) | 2010-06-02 |
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Country Status (8)
Country | Link |
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US (2) | US8241602B2 (ja) |
EP (2) | EP1445236A1 (ja) |
JP (1) | JP4474409B2 (ja) |
CN (1) | CN100393616C (ja) |
AT (1) | ATE413364T1 (ja) |
DE (1) | DE602004017573D1 (ja) |
ES (1) | ES2314369T3 (ja) |
WO (1) | WO2004069742A1 (ja) |
Families Citing this family (26)
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EP1428573B1 (de) * | 2002-12-03 | 2011-06-22 | FutureCarbon GmbH | Vorrichtung und Verfahren zum Herstellen von Kohlenstoff-Nanomaterial |
EP1445236A1 (fr) | 2003-02-05 | 2004-08-11 | Université de Liège | Procédé et installation pour la fabrication de nanotubes de carbone |
EP1919826B1 (en) * | 2005-08-29 | 2015-10-07 | University Of The Witwatersrand Johannesburg | Process and reactor for producing carbon nanotubes |
GB0611485D0 (en) * | 2006-06-09 | 2006-07-19 | Statoil Asa | Method |
EP2236460A4 (en) * | 2008-01-21 | 2012-01-11 | Nikkiso Co Ltd | METHOD FOR PRODUCING CARBON NANOTUBES |
WO2010016395A1 (ja) * | 2008-08-08 | 2010-02-11 | 株式会社 東芝 | ナノカーボン生成装置 |
WO2010095509A1 (ja) * | 2009-02-17 | 2010-08-26 | 学校法人 名城大学 | 複合材料の製造方法および製造装置 |
DE102010005560A1 (de) | 2010-01-22 | 2011-07-28 | Bayer MaterialScience AG, 51373 | Herstellung von CNT |
EP2500376A1 (de) | 2011-03-17 | 2012-09-19 | Basf Se | Antistatische oder elektrisch leitfähige Polyurethane |
EP2694435B1 (en) | 2011-04-04 | 2020-07-08 | LG Chem, Ltd. | Apparatus and method for continuously producing carbon nanotubes |
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RU2614966C2 (ru) * | 2015-09-17 | 2017-03-31 | Федеральное государственное унитарное предприятие "Центральный научно-исследовательский институт машиностроения" (ФГУП ЦНИИмаш) | Способ получения углеродных нанотрубок в сверхзвуковом потоке и устройство для его осуществления |
US10421061B2 (en) * | 2015-10-19 | 2019-09-24 | Hohai University | Preparation method of alumina-carbon nano tube composite powder material |
EP4292702A3 (en) | 2016-07-15 | 2024-04-17 | OneD Material, Inc. | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
WO2018022999A1 (en) | 2016-07-28 | 2018-02-01 | Seerstone Llc. | Solid carbon products comprising compressed carbon nanotubes in a container and methods of forming same |
WO2019187909A1 (ja) * | 2018-03-27 | 2019-10-03 | 戸田工業株式会社 | ロータリーキルン |
JP6734552B1 (ja) * | 2019-03-05 | 2020-08-05 | 戸田工業株式会社 | 触媒粒子及びそれを用いた水素製造方法 |
JP6923046B2 (ja) * | 2019-03-05 | 2021-08-18 | 戸田工業株式会社 | 触媒粒子及びそれを用いた水素製造方法 |
CN109928361B (zh) * | 2019-03-19 | 2020-10-09 | 中国矿业大学 | 一种具有自催化功能的碳纳米管兼氢气生产系统及方法 |
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IT1245346B (it) * | 1990-04-09 | 1994-09-20 | Blufin Spa | Metodo di preriscaldo rottame di ferro tramite pirolisi di residui resinosi in esso contenuti con recupero integrale del loro contenuto energetico e miglioramento del ciclo siderurgico |
FR2664506B1 (fr) * | 1990-07-13 | 1993-05-07 | Bp Chemicals Snc | Procede et dispositif d'introduction d'une poudre dans un reacteur. |
AUPN644895A0 (en) * | 1995-11-08 | 1995-11-30 | Miltox Holdings Pte Ltd | Method and apparatus for waste treatment |
FR2741363B1 (fr) | 1995-11-17 | 1998-02-20 | Carbone Ind | Procede et four d'activation d'une nappe textile tissee ou non tissee a base de fils continus ou de fils de fibres carbonees |
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2003
- 2003-02-05 EP EP03075349A patent/EP1445236A1/fr not_active Withdrawn
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- 2004-01-28 CN CNB2004800036065A patent/CN100393616C/zh not_active Expired - Lifetime
- 2004-01-28 EP EP04705814A patent/EP1594802B1/fr not_active Expired - Lifetime
- 2004-01-28 JP JP2006501709A patent/JP4474409B2/ja not_active Expired - Lifetime
- 2004-01-28 DE DE602004017573T patent/DE602004017573D1/de not_active Expired - Lifetime
- 2004-01-28 ES ES04705814T patent/ES2314369T3/es not_active Expired - Lifetime
- 2004-01-28 AT AT04705814T patent/ATE413364T1/de not_active IP Right Cessation
- 2004-01-28 WO PCT/EP2004/000952 patent/WO2004069742A1/fr active Search and Examination
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Also Published As
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US20070025906A1 (en) | 2007-02-01 |
CN1747894A (zh) | 2006-03-15 |
US20120269696A1 (en) | 2012-10-25 |
JP2006516946A (ja) | 2006-07-13 |
CN100393616C (zh) | 2008-06-11 |
US8241602B2 (en) | 2012-08-14 |
WO2004069742A1 (fr) | 2004-08-19 |
DE602004017573D1 (de) | 2008-12-18 |
ES2314369T3 (es) | 2009-03-16 |
EP1594802B1 (fr) | 2008-11-05 |
ATE413364T1 (de) | 2008-11-15 |
US8597587B2 (en) | 2013-12-03 |
EP1445236A1 (fr) | 2004-08-11 |
EP1594802A1 (fr) | 2005-11-16 |
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