EP1521863B1 - Procede de revetement de surfaces metalliques - Google Patents
Procede de revetement de surfaces metalliques Download PDFInfo
- Publication number
- EP1521863B1 EP1521863B1 EP03763755A EP03763755A EP1521863B1 EP 1521863 B1 EP1521863 B1 EP 1521863B1 EP 03763755 A EP03763755 A EP 03763755A EP 03763755 A EP03763755 A EP 03763755A EP 1521863 B1 EP1521863 B1 EP 1521863B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- concentration range
- range
- phosphating solution
- process according
- virtually none
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
- C23C22/364—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also manganese cations
- C23C22/365—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also manganese cations containing also zinc and nickel cations
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
- C23C22/362—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also zinc cations
Claims (15)
- Procédé de traitement ou de prétraitement de pièces, profilés, rubans, tôles et/ou fils, dotés de surfaces métalliques qui, pour au moins 5 % de ces surfaces, sont en aluminium et/ou en au moins un alliage d'aluminium, les autres surfaces métalliques pouvant, le cas échéant, être principalement en alliages de fer, en zinc et/ou en alliages de zinc, avec une solution aqueuse acide contenant des espèces fluorure, zinc et phosphate, lequel procédé est caractérisé en ce que les teneurs de la solution de phosphatation en espèces dissoutes sont comme suit :- la teneur en sodium est pratiquement nulle ou équivaut à une concentration d'au moins 0,04 g/L ;- la teneur en potassium est pratiquement nulle ou équivaut à une concentration d'au moins 0,025 g/L ;- la teneur totale en sodium et potassium équivaut à une concentration de 0,3 à 1,8 g/L de sodium, la teneur en potassium étant calculée en équivalents de sodium, sur la base du nombre de moles ;- la teneur en zinc équivaut à une concentration de 0,2 à 4 g/L ;- la teneur en phosphate, calculée en espèce PO4, équivaut à une concentration de 4 à 65 g/L ;- la teneur en fluorure libre équivaut à une concentration de 0,03 à 0,5 g/L ;- la teneur totale en fluorure équivaut à une concentration de 0,1 à 5 g/L ;- et le cas échéant, la teneur en nitrate vaut au moins 0,2 g/L ;et dans lequel procédé il n'y a, sur les surfaces en aluminium et/ou en au moins un alliage d'aluminium ainsi traitées par phosphatation, aucun ou presque aucun précipité à base de complexes de type aluminofluorure d'ammonium, de métal alcalin et/ou de métal alcalino-terreux qui se dépose, que ce soit sur la surface métallique, sous la couche de phosphate et/ou entre les cristaux de phosphate de zinc au sein de la couche de phosphate, mais il se dépose sur les surfaces métalliques une couche de phosphate contenant du zinc dont le poids surfacique vaut de 0,5 à 10 g/m2.
- Procédé conforme à la revendication 1, caractérisé en ce que la teneur de la solution de phosphatation en aluminium dissous équivaut à une concentration de 0,002 à 1 g/L.
- Procédé conforme à la revendication 1 ou 2, caractérisé en ce que la teneur totale de la solution de phosphatation en complexes de types silicofluorure et borofluorure, considérés ensemble, vaut de 0,01 à 8 g/L, teneur calculée, le cas échéant, en équivalents de l'espèce SiF6 sur la base du nombre de moles, étant entendu que ces deux types de fluorures complexes ne sont pas obligatoirement présents simultanément.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la teneur de la solution de phosphatation en espèces de type fluorure lié à l'état de complexe vaut de 0,01 à 8 g/L, teneur calculée en équivalents de l'espèce SiF6 sur la base du nombre de moles.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- du nickel en une teneur pratiquement nulle ou équivalant à une concentration de 0,001 à 3 g/L,- et/ou du manganèse en une teneur pratiquement nulle ou équivalant à une concentration de 0,002 à 5 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- des ions de fer Fe2+ dissous en une teneur pratiquement nulle ou équiva-lant à une concentration de 0,005 à 3 g/L,- et/ou des ions de fer Fe3+ complexés en une teneur pratiquement nulle ou équivalant à une concentration de 0,005 à 1 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- de l'argent en une teneur pratiquement nulle ou équivalant à une concentration de 0,001 à 0,080 g/L,- et/ou du cuivre en une teneur pratiquement nulle ou équivalant à une concentration de 0,001 à 0,050 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- du titane en une teneur pratiquement nulle ou équivalant à une concentration de 0,001 à 0,200 g/L,- et/ou du zirconium en une teneur pratiquement nulle ou équivalant à une concentration de 0,001 à 0,200 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- des ions ammonium en une teneur pratiquement nulle ou équivalant à une concentration de 0,01 à 50 g/L,- et/ou des ions nitrate en une teneur pratiquement nulle ou équivalant à une concentration de 0,01 à 30 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient à l'état dissous :- des ions sulfate en une teneur pratiquement nulle ou équivalant à une concentration de 0,005 à 5 g/L,- et/ou des ions chlorure en une teneur pratiquement nulle ou équivalant à une concentration de 0,020 à 0,5 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la solution de phosphatation contient au moins un accélérateur choisi dans l'ensemble formé par les composés ou ions à base :- de composés azotés, en une concentration de 0,01 à 8 g/L,- de chlorate, en une concentration de 0,01 à 6 g/L,- d'hydroxylamine, en une concentration de 0,01 à 3 g/L,- ou de peroxyde, y compris les peroxydes organiques hydrosolubles, en une concentration, calculée en équivalents de H2O2, de 0,001 à 0,200 g/L,et présent en une teneur équivalant à une concentration située dans l'intervalle indiqué.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la teneur de la solution de phosphatation en magnésium vaut au plus 1 g/L, et de préférence, au plus 0,15 g/L.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que l'on maintient le pH dans l'intervalle allant de 2 à 4.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que la teneur en acide libre après saturation au chlorure de potassium vaut de 0,3 à 6 points, la teneur totale en acide après dilution vaut de 8 à 70 points, et/ou la teneur totale en acide selon Fischer vaut de 4 à 50 points.
- Procédé conforme à l'une des revendications précédentes, caractérisé en ce que le revêtement de phosphate est déposé à une température de 20 à 70 °C.
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2002131279 DE10231279B3 (de) | 2002-07-10 | 2002-07-10 | Verfahren zur Beschichtung von metallischen Oberflächen und Verwendung der derart beschichteten Substrate |
DE10231279 | 2002-07-10 | ||
DE10236526 | 2002-08-09 | ||
DE2002136526 DE10236526A1 (de) | 2002-08-09 | 2002-08-09 | Verfahren zur Beschichtung von metallischen Oberflächen |
PCT/EP2003/007359 WO2004007799A2 (fr) | 2002-07-10 | 2003-07-09 | Procede de revetement de surfaces metalliques |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1521863A2 EP1521863A2 (fr) | 2005-04-13 |
EP1521863B1 true EP1521863B1 (fr) | 2008-06-25 |
Family
ID=30116625
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP03763755A Expired - Lifetime EP1521863B1 (fr) | 2002-07-10 | 2003-07-09 | Procede de revetement de surfaces metalliques |
Country Status (11)
Country | Link |
---|---|
US (2) | US20050205166A1 (fr) |
EP (1) | EP1521863B1 (fr) |
JP (1) | JP4233565B2 (fr) |
CN (1) | CN100374620C (fr) |
AT (1) | ATE399218T1 (fr) |
AU (1) | AU2003250917A1 (fr) |
CA (1) | CA2494559C (fr) |
DE (1) | DE50310042D1 (fr) |
ES (1) | ES2309349T3 (fr) |
PT (1) | PT1521863E (fr) |
WO (1) | WO2004007799A2 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102022106091A1 (de) | 2022-03-16 | 2023-09-21 | Thyssenkrupp Steel Europe Ag | Verfahren zum Modifizieren einer Oberfläche eines beschichteten Stahlblechs |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102005023023B4 (de) * | 2005-05-19 | 2017-02-09 | Chemetall Gmbh | Verfahren zur Vorbereitung von metallischen Werkstücken zum Kaltumformen, mit dem Verfahren beschichtete Werkstücke und ihre Verwendung |
DE102006052919A1 (de) * | 2006-11-08 | 2008-05-15 | Henkel Kgaa | Zr-/Ti-haltige Phosphatierlösung zur Passivierung von Metallverbundoberflächen |
DE102008000600B4 (de) * | 2008-03-11 | 2010-05-12 | Chemetall Gmbh | Verfahren zur Beschichtung von metallischen Oberflächen mit einem Passivierungsmittel, das Passivierungsmittel, die hiermit erzeugte Beschichtung und ihre Verwendung |
CN101575703A (zh) * | 2008-05-09 | 2009-11-11 | 日本轻金属株式会社 | 表面处理铝材的制造方法、表面处理铝材及铝材的表面处理方法 |
DE102010030697A1 (de) * | 2010-06-30 | 2012-01-05 | Henkel Ag & Co. Kgaa | Verfahren zur selektiven Phosphatierung einer Verbundmetallkonstruktion |
DE102011100974A1 (de) * | 2011-05-09 | 2012-11-15 | Knorr-Bremse Systeme für Schienenfahrzeuge GmbH | Schienenrad und Verfahren zur Herstellung eines Schienenrades |
CN105331966B (zh) | 2015-11-30 | 2018-04-27 | 宝山钢铁股份有限公司 | 一种无铬表面处理镀锡板、其生产方法及表面处理剂 |
US11518960B2 (en) | 2016-08-24 | 2022-12-06 | Ppg Industries Ohio, Inc. | Alkaline molybdenum cation and phosphonate-containing cleaning composition |
HUE047403T2 (hu) | 2017-04-21 | 2020-04-28 | Henkel Ag & Co Kgaa | Lerakódásmentes foszfátbevonat-képzési módszer fémalkatrész sorozatokhoz |
EP3392376A1 (fr) | 2017-04-21 | 2018-10-24 | Henkel AG & Co. KGaA | Procédé formant des couches de phosphatate de zinc sur des composants métalliques en série |
KR102655537B1 (ko) * | 2017-12-12 | 2024-04-09 | 케메탈 게엠베하 | 빙정석을 함유하는 침착물을 제거하기 위한 무-붕산 조성물 |
JP7443253B2 (ja) * | 2018-02-19 | 2024-03-05 | ケメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング | 複合金属構造体の選択的リン酸塩処理方法 |
CN112442699A (zh) * | 2019-08-29 | 2021-03-05 | 晟通科技集团有限公司 | 表面清洗剂 |
KR102456800B1 (ko) * | 2021-07-05 | 2022-10-21 | 삼양화학산업 주식회사 | 친환경 표면처리제가 적용된 연속 도장처리방법 |
Family Cites Families (29)
Publication number | Priority date | Publication date | Assignee | Title |
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US2375468A (en) | 1938-02-04 | 1945-05-08 | Parker Rust Proof Co | Phosphate coating of metals |
DE977633C (de) | 1950-07-06 | 1967-11-02 | Galvapol Ges Fuer Galvanotechn | Verfahren zur Herstellung von Phosphatueberzuegen auf eisenhaltigen Metallgegenstaenden |
US3619300A (en) * | 1968-11-13 | 1971-11-09 | Amchem Prod | Phosphate conversion coating of aluminum, zinc or iron |
US3676224A (en) | 1970-10-16 | 1972-07-11 | Lubrizol Corp | Phosphating solution with scale suppressing characteristics |
JPS5339945A (en) | 1976-09-25 | 1978-04-12 | Nippon Packaging Kk | Surface treatment of zinc or zinc alloy |
GB2080835B (en) | 1980-07-25 | 1984-08-30 | Pyrene Chemical Services Ltd | Prevention of sludge in phosphating baths |
GB2148950B (en) | 1983-10-26 | 1987-02-04 | Pyrene Chemical Services Ltd | Phosphating composition and processes |
DE3800835A1 (de) | 1988-01-14 | 1989-07-27 | Henkel Kgaa | Verfahren zur phosphatierung von metalloberflaechen |
US5200000A (en) * | 1989-01-31 | 1993-04-06 | Nihon Parkerizing Co., Ltd. | Phosphate treatment solution for composite structures and method for treatment |
DE3920296A1 (de) | 1989-06-21 | 1991-01-10 | Henkel Kgaa | Verfahren zur herstellung von mangan- und magnesiumhaltigen zinkphosphatueberzuegen |
KR100197145B1 (ko) | 1989-12-19 | 1999-06-15 | 후지이 히로시 | 금속표면의 인산아연 처리방법 |
JP2695963B2 (ja) | 1990-03-16 | 1998-01-14 | マツダ株式会社 | 金属表面のリン酸塩処理方法 |
JPH07100870B2 (ja) | 1990-04-24 | 1995-11-01 | 日本ペイント株式会社 | 金属表面のリン酸亜鉛皮膜処理方法 |
DE4306446A1 (de) | 1993-03-02 | 1994-09-08 | Metallgesellschaft Ag | Verfahren zur Erleichterung der Kaltumformung |
JPH0820876A (ja) * | 1994-07-12 | 1996-01-23 | Nippon Parkerizing Co Ltd | リン酸塩化成処理方法 |
CN1093891C (zh) * | 1994-12-06 | 2002-11-06 | 日本帕卡濑精株式会社 | 含水磷酸锌化学转化处理液及处理金属材料的方法 |
DE19544614A1 (de) * | 1995-11-30 | 1997-06-05 | Metallgesellschaft Ag | Verfahren zur Phospatierung von Metalloberflächen |
DE19634685A1 (de) | 1996-08-28 | 1998-03-05 | Metallgesellschaft Ag | Wässrige Lösung und Verfahren zur Phosphatierung metallischer Oberflächen |
DE59805918D1 (de) | 1997-08-06 | 2002-11-14 | Henkel Kgaa | Mit n-oxiden beschleunigtes phosphatierverfahren |
DE19808440C2 (de) * | 1998-02-27 | 2000-08-24 | Metallgesellschaft Ag | Wässrige Lösung und Verfahren zur Phosphatierung metallischer Oberflächen sowie eine Verwendung der Lösung und des Verfahrens |
DE19834796A1 (de) | 1998-08-01 | 2000-02-03 | Henkel Kgaa | Verfahren zur Phosphatierung, Nachspülung und kathodischer Elektrotauchlackierung |
DE19958192A1 (de) | 1999-12-02 | 2001-06-07 | Henkel Kgaa | Verfahren zur Phosphatierung, Nachspülung und kathodischer Elektrotauchlackierung |
DE10026850A1 (de) | 2000-05-31 | 2001-12-06 | Chemetall Gmbh | Verfahren zum Behandeln bzw. Vorbehandeln von Bauteilen mit Aluminium-Oberflächen |
US6530999B2 (en) | 2000-10-10 | 2003-03-11 | Henkel Corporation | Phosphate conversion coating |
DE10110834B4 (de) | 2001-03-06 | 2005-03-10 | Chemetall Gmbh | Verfahren zur Beschichtung von metallischen Oberflächen und Verwendung der derart beschichteten Substrate |
DE10110833B4 (de) | 2001-03-06 | 2005-03-24 | Chemetall Gmbh | Verfahren zum Aufbringen eines Phosphatüberzuges und Verwendung der derart phosphatierten Metallteile |
DE10118552A1 (de) | 2001-04-14 | 2002-10-17 | Henkel Kgaa | Bestimmung der Beschleunigerkonzentration in Phosphatierbäder |
DE10155976A1 (de) | 2001-11-14 | 2003-05-22 | Henkel Kgaa | Steuerung der Beschleunigerkonzentration in Phosphatierbäder |
DE10320313B4 (de) | 2003-05-06 | 2005-08-11 | Chemetall Gmbh | Verfahren zum Beschichten von metallischen Körpern mit einer Phosphatierungslösung, Phosphatierungslösung und die Verwendung des beschichteten Gegenstandes |
-
2003
- 2003-07-09 AT AT03763755T patent/ATE399218T1/de active
- 2003-07-09 ES ES03763755T patent/ES2309349T3/es not_active Expired - Lifetime
- 2003-07-09 PT PT03763755T patent/PT1521863E/pt unknown
- 2003-07-09 JP JP2005505061A patent/JP4233565B2/ja not_active Expired - Fee Related
- 2003-07-09 CN CNB03816065XA patent/CN100374620C/zh not_active Expired - Fee Related
- 2003-07-09 DE DE50310042T patent/DE50310042D1/de not_active Expired - Lifetime
- 2003-07-09 AU AU2003250917A patent/AU2003250917A1/en not_active Abandoned
- 2003-07-09 US US10/519,006 patent/US20050205166A1/en not_active Abandoned
- 2003-07-09 EP EP03763755A patent/EP1521863B1/fr not_active Expired - Lifetime
- 2003-07-09 CA CA2494559A patent/CA2494559C/fr not_active Expired - Fee Related
- 2003-07-09 WO PCT/EP2003/007359 patent/WO2004007799A2/fr active IP Right Grant
-
2011
- 2011-04-06 US US13/080,974 patent/US8349092B2/en not_active Expired - Lifetime
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102022106091A1 (de) | 2022-03-16 | 2023-09-21 | Thyssenkrupp Steel Europe Ag | Verfahren zum Modifizieren einer Oberfläche eines beschichteten Stahlblechs |
Also Published As
Publication number | Publication date |
---|---|
US20110198000A1 (en) | 2011-08-18 |
AU2003250917A8 (en) | 2004-02-02 |
JP2006501372A (ja) | 2006-01-12 |
WO2004007799A2 (fr) | 2004-01-22 |
DE50310042D1 (de) | 2008-08-07 |
WO2004007799A3 (fr) | 2004-04-08 |
US20050205166A1 (en) | 2005-09-22 |
US8349092B2 (en) | 2013-01-08 |
ES2309349T3 (es) | 2008-12-16 |
EP1521863A2 (fr) | 2005-04-13 |
CN100374620C (zh) | 2008-03-12 |
JP4233565B2 (ja) | 2009-03-04 |
AU2003250917A1 (en) | 2004-02-02 |
PT1521863E (pt) | 2008-09-19 |
CA2494559C (fr) | 2011-09-20 |
CA2494559A1 (fr) | 2004-01-22 |
CN1665957A (zh) | 2005-09-07 |
ATE399218T1 (de) | 2008-07-15 |
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