EP1472380A2 - Blech aus al-si-mg-legierung für karroserie von kraftfahrzeugen - Google Patents
Blech aus al-si-mg-legierung für karroserie von kraftfahrzeugenInfo
- Publication number
- EP1472380A2 EP1472380A2 EP03712292A EP03712292A EP1472380A2 EP 1472380 A2 EP1472380 A2 EP 1472380A2 EP 03712292 A EP03712292 A EP 03712292A EP 03712292 A EP03712292 A EP 03712292A EP 1472380 A2 EP1472380 A2 EP 1472380A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- sheet according
- mpa
- elastic limit
- sheet
- temperature
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
Definitions
- the invention relates to the field of sheets of Al-Si-Mg alloy, more particularly of type 6016 alloy according to the designation of the Aluminum Association, intended for the manufacture by stamping of parts of car body skin, such as fenders, doors, tailgates, hoods or roofs.
- Aluminum is increasingly used in automobile construction to reduce the weight of vehicles and thereby reduce fuel consumption and the emission of pollutants and greenhouse gases.
- the sheets are used in particular for the manufacture of body skin parts, in particular the openings.
- This type of application requires a set of properties, sometimes antagonistic such as: high formability for stamping and crimping operations, - a limit of elasticity controlled in the delivery state of the sheet to control elastic return , high mechanical resistance after curing the paints to obtain good resistance to indentation while minimizing the weight of the part, good resistance to corrosion, in particular filiform corrosion, of the painted part, good surface quality after shaping and painting,
- alloys of the 6000 series that is to say the alloys of the 6000 series.
- alloys 6016 and 6016A with thicknesses of the order of 1 to 1.2 mm, are the most used for this application, because they lead to a better compromise between the various properties required, in particular ensuring better formability, in particular for crimping, and better resistance to filiform corrosion than alloys with a content of higher copper such as 6111 widely used in the United States.
- Alloys of type 6016 are described in particular in patents FR 2360684 of Alusuisse and EP 0259232 of the applicant, while alloys of type 6111 are described in US patent 4,614,552 of Alcan International Ltd.
- alloys with a low iron content such as those described in US Patents 5,525,169 and US 5,919,323 of Alcoa, and an alloy of this type has been registered as 6022
- Table 1 The compositions (% by weight of main elements) of alloys 6016, 6016 A, 6022 and 6111 registered with the Aluminum Association are indicated in table 1:
- the object of the present invention is to provide 6016 type alloy sheets for automotive body skin having a composition suitable for recycling, sufficient formability for deep drawing and crimping under severe conditions, improved indentation resistance compared to sheets of the prior art type 6016, while controlling elastic return, good bonding ability, cutting without formation of flakes, and good resistance to filiform corrosion.
- the subject of the invention is a sheet for a part of the skin of a car body, of thickness between 0.8 and 1.2 mm, of composition (% by weight): Fe: 0.25 - 0.40 and of preference: 0.25 - 0.35 If: 0.90 - 1.20 "" 0.95 - 1.10 Cu: 0.10 - 0.25 "" 0.15 - 0.20
- Mn 0.05 - 0.20 "" 0.08 - 0.15 other elements ⁇ 0.05 each and ⁇ 0.15 in total, aluminum residue, presenting after dissolution, quenching, pre-annealing or reversion, and maturation at room temperature between 3 weeks and 6 months, an elastic limit in the sense LR 0j2 of less than 160 MPa, and preferably less than 150 MPa.
- the elastic limit of the stamped part after a heat treatment corresponding to the curing of the paints is greater than 180 MPa, and preferably 200 MPa. Description of the invention
- the invention is based on a narrow field of composition within the composition of 6016A registered with the Aluminum Association, making it possible to obtain all of the properties sought.
- the silicon content is in the lower part of the 6016A content range, while the magnesium content remains in the center of the range. This lowering of the silicon content contributes to a more complete dissolution of the alloy, favorable to formability.
- the iron content remains above 0.25%, which authorizes, unlike low iron grades like 6022, the use of recycled metal, and is rather favorable to the surface appearance after stamping.
- the copper content is controlled within very narrow limits: a content of at least 0.1%, a little higher than that of the existing grades of 6016 or 6022, contributes to the mechanical resistance, but above 0, 25% of the alloy presents a risk of filiform corrosion.
- the alloy must contain at least 0.05% manganese, chromium, vanadium or zirconium to control the size of the grain, and avoid the appearance of orange peel during severe deformations, such as the crimp used for the covers. Conversely, a total content of these elements greater than 0.20% is unfavorable to formability.
- the method of manufacturing sheets according to the invention typically comprises the casting of a plate, possibly scalping of this plate, and its homogenization or a simple reheating at a temperature between 400 and 570 ° C with a duration between 6 and 24h.
- Hot rolling is preferably done at an inlet temperature above 510 ° C, which contributes to improving the mechanical strength compared to a lower inlet temperature.
- the winding temperature of the hot-rolled strip must be less than 350 ° C, and preferably less than 300 ° C, to guarantee the mechanical characteristics and to avoid line defect.
- the hot-rolled strip is then cold-rolled to the final thickness, possibly with intermediate annealing at a temperature between 300 and 450 ° C if it is carried out in a batch oven, or between 350 and 570 ° C s 'it is performed continuously.
- the last cold rolling pass can be carried out with a textured cylinder, for example by electron beam treatment (EBT), EDM or beam laser, which improves the formability and surface appearance of the part formed after painting.
- EBT electron beam treatment
- EDM electron beam laser
- Dissolution takes place at a temperature above the alloy's solvent temperature, while avoiding burns.
- the composition according to the invention makes it possible to carry out a very complete dissolution, resulting in an almost absence of silicon-type phases in the microstructure and in a very small peak area, of less than 1 J / g, in the range 565-580 ° C of a differential enthalpy analysis diagram, the test being carried out with a temperature rise rate of 20 ° C / min.
- the sheet in solution is then quenched, generally with cold water or air.
- the quenching can be immediately followed by a heat treatment of the pre-annealed type as described in the prior art mentioned above, intended to improve the performance of the hardening during the curing of the paints.
- Pre-tempering is not necessarily isothermal and its duration depends on the temperature. To take this into account, we can define an equivalent time t eq by the formula:
- T (in ° K) is the temperature and t the duration of the pre-tempering, T re f being a reference temperature of 373 ° K, or 100 ° C.
- pre-tempering to be effective, must be carried out at a temperature above 50 ° C. with an equivalent time of between 0.3 and 20 h. If the equivalent time is insufficient, the hardening kinetics when the paints are cured decreases with the waiting time at room temperature. If, on the contrary, the equivalent time is too high, the mechanical characteristics increase too much during pre-tempering, and the formability of the sheet degrades.
- an equivalent time 1 to 10 h, and preferably 3 to 6 h, is well suited.
- the sheet is most often stored at this stage for a more or less long time, which leads to natural maturation which increases the elastic limit over time.
- the sheets according to the invention After 3 weeks of maturation, the sheets according to the invention have, at a thickness of the order of 0.9 to 1 mm, an elastic limit L direction of the order of
- the sheet can be, before shaping, coated with a lubricant, oil or dry lubricant, suitable for stamping, assembly and surface treatment of the part to be produced.
- the sheets according to the invention have a formability, measured by the parameter
- the LDH parameter is widely used for the evaluation of the deep drawing of thick sheets 0.5 to 2 mm. It has been the subject of numerous publications, notably that of R. Thompson, "The LDH test to evaluate sheet metal formabiblity - Final Report of the LDH Committee of the North American Deep Drawing Research Group", SAE conference, Detroit, 1993, SAE Papern ° 930815.
- the LDH test is a blank stamping test blocked at the periphery by a rod. The pressure of the blank holder is controlled to avoid slipping in the rod. The blank, size 120 x 160 mm, is stressed in a mode close to plane deformation.
- Lubrication between the punch and the sheet is ensured by a plastic film and grease (Shell HDM2 grease).
- the lowering speed of the punch is 50 mm / min.
- the LDH value is the displacement of the break punch, i.e. the limit depth of the stamping.
- the average is established between three tests, giving a 95% confidence interval on the measurement of ⁇ 0.2 mm.
- the sheets according to the invention have a better crimpability than that of sheets of alloy 6111 or 6022 and as good as sheets of alloy 6016 of high strength of the prior art. This crimpability is evaluated by a laboratory test comprising a 90 ° drop, a 45 ° pre-crimp and a final flat crimp.
- the sheets according to the invention also have a very low deformation anisotropy, which can be measured by the difference between the LDH for a main deformation parallel to the direction of rolling, and a main deformation ⁇ perpendicular to the rolling direction. This difference is less than 1 mm, and preferably less than 0.6 mm.
- the bodywork piece of skin is generally produced by cutting a blank in the sheet, stamping this blank and trimming with the press.
- lineage ("roping” or “ridging” in English), which is detrimental to the appearance after painting, and can reduce formability, especially in case of strong deformation in the direction perpendicular to the rolling direction.
- Different means have been proposed in this sense, for example controlling the outlet temperature of hot rolling between 270 and 340 ° C, as indicated in patent EP 0259232 of the applicant.
- the design of the cutting tool is important in this regard, and recommendations were made in the article by D. Daniel et al. cited above.
- the part is covered with one or more layers of paint, each with a baking step.
- the critical step is the baking of the cataphoresis layer, which is generally done at a temperature between 150 and 200 ° C, for 15 to 30 minutes. In the absence of cataphoresis, the cooking temperature rarely exceeds 170 ° C.
- the firing of the paintings plays the role of an income treatment of the room.
- the elastic limit of the part produced with a sheet according to the invention, with baking for 20 min at 165 ° C., is greater than 180 MPa, and more often than 200 MPa. This gives a resistance to indentation with a part made from a 0.9 mm thick sheet dynamic comparable to that of a part produced from a sheet of steelwork of typical bodywork of elastic limit of the order of 250 to 300 MPa and thickness
- the sheets according to the invention make it possible to carry out the various operations commonly used for the manufacture of car body skin parts, such as crimping, clinching, riveting, spot welding, laser welding and bonding.
- crimped joints used in particular in the manufacture of covers, without first applying a chemical treatment to the surfaces such as chemical conversion or passivation, for example using compounds phosphochromic, or products based on titanium, zirconium or silanes.
- the parts produced from sheets according to the invention also exhibit, after painting, good resistance to filiform corrosion, better than that of high copper alloys such as 6111.
- high copper alloys such as 6111.
- the major difficulty lies in the management of the differences in thermal expansion between the two materials during the curing of the paints, in particular during the curing of cataphoresis which generally takes place between 160 and 200 ° C. . Indeed, it is essential to limit the residual deformation after baking to an acceptable level for the appearance of the vehicle.
- the sheets according to the invention make it possible to limit these deformations. Indeed, the Applicant has demonstrated that a high elastic limit at the firing temperature, for example greater than 140 MPa at a temperature of 160 ° C for the alloy according to the invention, had a favorable effect on the level of deformation, if the assembly is carried out after cooking, the temperature of which is preferable. Other factors can also limit deformations, for example the presence of ribs intended to stiffen the aluminum panel, or the spacing of the assembly points. You can also use an assembly with continuous connection like gluing, with at least partial polymerization of the glue before baking, or laser welding by transparency.
- Composition A represents a classic 6016
- B corresponds to that of the applicant's DR100 grade described in the articles mentioned above
- C and D correspond to an alloy 6111
- E corresponds to an alloy 6022
- F, G, H and I have neighboring compositions, differing either by Cu (F) or by Mn (G and H) from composition I according to the invention.
- the plates were scalped, homogenized for 10 h at 570 ° C, then hot-rolled directly on heat of homogenization, first on a reversible dammer, then on a tandem rolling mill.
- the rolling start temperature was of the order of
- the elastic limit R 0> 2 directions L was measured after 3 weeks and 6 months of maturation respectively at room temperature, then after a 30 min tempering treatment at 165 ° C or 185 ° C , simulating the baking treatment of paints.
- the formability was also measured using the LDH parameter (in mm), the main deformation being respectively parallel and perpendicular to the direction of rolling. The results are shown in Table 2:
- sample I according to the invention exhibits, after 3 weeks maturation, an elastic limit of the same order as that of the conventional 6016
- the formability, measured by the LDH parameter, is practically as good as that of the best alloy, that is to say the DR100.
- the crimping behavior in the direction parallel to rolling and in the perpendicular direction, the resistance to filiform corrosion after phosphating, cataphoresis and painting, as well as the appearance or no glitter or filaments during cutting or trimming after stamping.
- the crimping test is carried out in 3 operations: dropping the edges at 90 ° C, pre-crimping at 45 ° and crimping flat on a sheet of liner 0.7 mm thick. The crimped edges are then classified by visual inspection, as indicated in the article by D. Daniel et al. to IBEC 99. The resistance to filiform corrosion is assessed according to standard EN 3665, with samples of dimension 150 x 60 x 1 mm painted and scratched. The test procedure includes activation of HCl vapor corrosion for 1 h, then exposure in a humid chamber at 40 ° C for 1000 h.
- Aluminum alloy panels of the composition indicated in Table 4 were manufactured, with a manufacturing range similar to that of Example 1, with or without pre-tempering and heat treatment after shaping and before assembly, as also shown in table 4.
- the size of the panels is 1.6 mx 0.9 m.
- the alloy according to the invention makes it possible to reduce the residual deformations after baking.
- the performance of the alloys is well correlated with the yield strength at the baking temperature.
- a heat treatment before assembly and the addition of ribs are beneficial in reducing deformation.
- the resistance to dynamic indentation of a sheet of thickness 1 mm developed with a manufacturing range of the type of that of Example 1, comprising a pre-tempering equivalent time 5 h, and a heat treatment was evaluated. of 20 min at different temperatures simulating a baking of the paints, an alloy according to the invention and a 6016 DR100 alloy, in comparison with that of a steel sheet of elastic limit 290 MPa after curing the paints, of thickness 0 , 7 mm.
- This value of 290 MPa after baking for the elastic limit of a body steel sheet corresponds approximately to the average of the elastic limits of the steel sheets used for the skin skins of the most common recent European cars. .
- a thickness of 1 mm for an aluminum sheet represents an elongation of about 50% compared to a steel sheet 0.7 mm thick.
- the device used for the indentation test comprises an indentor with a diameter of 15 mm and a weight of 138 g, dropped from a height of 1 m, at a speed of about 16 km / h, on the sample of sheet metal clamped between two steel plates. The depth of permanent indentation is measured (in mm). The results are shown in Table 6.
- the sheet of thickness 1 mm according to the invention has the same resistance to indentation as that of steel sheet 0.7 mm.
- the DR100 alloy this is only true for a paint curing temperature of 205 ° C, higher than the temperatures usually used by car manufacturers.
- a more resistant alloy such as 6111 would increase the resistance to indentation beyond the needs of the market, but at the expense of formability, especially during crimping.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0201346A FR2835533B1 (fr) | 2002-02-05 | 2002-02-05 | TOLE EN ALLIAGE Al-Si-Mg POUR PEAU DE CARROSSERIE AUTOMOBILE |
FR0201346 | 2002-02-05 | ||
PCT/FR2003/000318 WO2003066919A2 (fr) | 2002-02-05 | 2003-02-03 | Tole en alliage al-si-mg pour peau de carrosserie automobile |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1472380A2 true EP1472380A2 (de) | 2004-11-03 |
EP1472380B1 EP1472380B1 (de) | 2008-11-05 |
Family
ID=27619894
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP03712292A Revoked EP1472380B1 (de) | 2002-02-05 | 2003-02-03 | Blech aus al-si-mg-legierung für karroserie von kraftfahrzeugen |
Country Status (11)
Country | Link |
---|---|
US (1) | US20050028894A1 (de) |
EP (1) | EP1472380B1 (de) |
JP (2) | JP2005525462A (de) |
KR (1) | KR100964855B1 (de) |
AT (1) | ATE413476T1 (de) |
AU (1) | AU2003216971A1 (de) |
CA (1) | CA2471501C (de) |
DE (2) | DE60324526D1 (de) |
ES (1) | ES2316738T3 (de) |
FR (1) | FR2835533B1 (de) |
WO (1) | WO2003066919A2 (de) |
Families Citing this family (28)
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DE10324452B4 (de) * | 2002-07-01 | 2010-05-06 | Aleris Aluminum Duffel Bvba | AI-Mg-Si-Legierungsblech |
EP1533394A1 (de) | 2003-11-20 | 2005-05-25 | Alcan Technology & Management Ltd. | Automobilkarosseriebauteil |
US8109535B2 (en) * | 2004-12-13 | 2012-02-07 | Ford Global Technologies | Sport utility vehicle (SUV) frame architecture for improved vehicle-to-vehicle compatibility |
EP2156945A1 (de) | 2008-08-13 | 2010-02-24 | Novelis Inc. | Plattiertes Kraftfahrzeug-Blechprodukt |
CN103180471B (zh) * | 2010-11-05 | 2016-01-13 | 阿莱利斯铝业迪弗尔私人有限公司 | 由轧制的Al-Zn合金制造汽车结构部件的方法 |
US9938612B2 (en) | 2013-03-07 | 2018-04-10 | Aleris Aluminum Duffel Bvba | Method of manufacturing an Al—Mg—Si alloy rolled sheet product with excellent formability |
US10150354B2 (en) * | 2014-02-21 | 2018-12-11 | Ford Global Technologies, Llc | Automotive door structure for sail mounted mirrors |
EP3699309B1 (de) | 2014-10-28 | 2023-12-27 | Novelis Inc. | Aluminiumlegierungsprodukte und verfahren zur herstellung |
ES2900103T3 (es) | 2015-01-12 | 2022-03-15 | Novelis Inc | Lámina de aluminio para automóviles altamente conformable con estriado superficial reducido o ausente y procedimiento de preparación |
MX2017014219A (es) | 2015-05-08 | 2018-03-01 | Novelis Inc | Tratamiento termico por choque de articulos de aleacion de aluminio. |
FR3038242B1 (fr) * | 2015-07-02 | 2017-06-23 | Constellium Neuf-Brisach | Alliage d'aluminium pour soudage par laser sans fils d'apport |
AU2016369546B2 (en) | 2015-12-18 | 2019-06-13 | Novelis Inc. | High strength 6xxx aluminum alloys and methods of making the same |
WO2018075353A1 (en) | 2016-10-17 | 2018-04-26 | Novelis Inc. | Metal sheet with tailored properties |
EP3532213B1 (de) | 2016-10-27 | 2021-09-01 | Novelis, Inc. | Vorrichtung und verfahren zur herstellung von dicken aluminiumlegierungsartikeln |
CA3041580A1 (en) | 2016-10-27 | 2018-05-03 | Novelis Inc. | High strength 7xxx series aluminum alloys and methods of making the same |
BR112019007379B1 (pt) | 2016-10-27 | 2022-11-08 | Novelis Inc | Método para produzir um produto de liga de alumínio, e, produto de liga de alumínio |
US10428412B2 (en) * | 2016-11-04 | 2019-10-01 | Ford Motor Company | Artificial aging of strained sheet metal for strength uniformity |
JP7025428B2 (ja) | 2016-12-16 | 2022-02-24 | ノベリス・インコーポレイテッド | 自然時効硬化に耐性のある高強度および高成形性のアルミニウム合金ならびにその作製方法 |
KR102253860B1 (ko) | 2016-12-16 | 2021-05-24 | 노벨리스 인크. | 알루미늄 합금 및 그 제조 방법 |
FR3060606B1 (fr) * | 2016-12-19 | 2018-12-07 | Constellium Neuf-Brisach | Alliage d’aluminium pour soudage par laser sans fil d’apport |
FR3065013B1 (fr) * | 2017-04-06 | 2020-08-07 | Constellium Neuf-Brisach | Procede ameliore de fabrication de composant de structure de caisse automobile |
CN110662852A (zh) | 2017-05-26 | 2020-01-07 | 诺维尔里斯公司 | 高强度耐腐蚀6xxx系列铝合金和其制造方法 |
MX2020011510A (es) | 2018-05-15 | 2020-12-07 | Novelis Inc | Aleaciones de aluminio 6xxx y 7xxx de alta resistencia y metodos para llevarlos a cabo. |
CA3106316C (en) | 2018-07-23 | 2023-01-17 | Novelis Inc. | Methods of making highly-formable aluminum alloys and aluminum alloy products thereof |
CN111334728B (zh) * | 2018-12-19 | 2022-04-05 | 有研工程技术研究院有限公司 | 一种改善铝合金板材翻边性能的方法 |
CA3126851A1 (en) | 2019-03-13 | 2020-09-17 | Novelis Inc. | Age-hardenable and highly formable aluminum alloys, monolithic sheet made therof and clad aluminum alloy product comprising it |
EP3839085B1 (de) * | 2019-12-17 | 2023-04-26 | Constellium Neuf-Brisach | Verbessertes verfahren zur herstellung eines strukturteils für eine kraftfahrzeugkarosserie |
CN115485469A (zh) | 2020-02-14 | 2022-12-16 | 康明斯有限公司 | 使用发动机转速传感器进行失火检测的设备、方法、系统和技术 |
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JPS6289852A (ja) * | 1985-09-24 | 1987-04-24 | Kobe Steel Ltd | 焼付硬化性に優れたアルミニウム合金板の製造法 |
FR2601040B1 (fr) * | 1986-07-07 | 1988-09-02 | Cegedur | Alliage d'aluminium chaudronnable et soudable et son procede de fabrication |
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US5919323A (en) * | 1994-05-11 | 1999-07-06 | Aluminum Company Of America | Corrosion resistant aluminum alloy rolled sheet |
JPH0931616A (ja) * | 1995-07-21 | 1997-02-04 | Nippon Steel Corp | 成形性に優れたAl−Mg−Si系合金板とその製造方法 |
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-
2002
- 2002-02-05 FR FR0201346A patent/FR2835533B1/fr not_active Expired - Fee Related
-
2003
- 2003-02-03 AT AT03712292T patent/ATE413476T1/de not_active IP Right Cessation
- 2003-02-03 KR KR1020047012157A patent/KR100964855B1/ko not_active IP Right Cessation
- 2003-02-03 DE DE60324526T patent/DE60324526D1/de not_active Expired - Lifetime
- 2003-02-03 AU AU2003216971A patent/AU2003216971A1/en not_active Abandoned
- 2003-02-03 EP EP03712292A patent/EP1472380B1/de not_active Revoked
- 2003-02-03 US US10/502,659 patent/US20050028894A1/en not_active Abandoned
- 2003-02-03 ES ES03712292T patent/ES2316738T3/es not_active Expired - Lifetime
- 2003-02-03 CA CA2471501A patent/CA2471501C/fr not_active Expired - Fee Related
- 2003-02-03 JP JP2003566264A patent/JP2005525462A/ja active Pending
- 2003-02-03 WO PCT/FR2003/000318 patent/WO2003066919A2/fr active Application Filing
- 2003-02-03 DE DE03712292T patent/DE03712292T1/de active Pending
-
2008
- 2008-12-09 JP JP2008312816A patent/JP2009133006A/ja active Pending
Non-Patent Citations (1)
Title |
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See references of WO03066919A2 * |
Also Published As
Publication number | Publication date |
---|---|
CA2471501A1 (fr) | 2003-08-14 |
EP1472380B1 (de) | 2008-11-05 |
ES2316738T3 (es) | 2009-04-16 |
AU2003216971A1 (en) | 2003-09-02 |
DE60324526D1 (de) | 2008-12-18 |
JP2005525462A (ja) | 2005-08-25 |
FR2835533A1 (fr) | 2003-08-08 |
WO2003066919A3 (fr) | 2004-04-08 |
JP2009133006A (ja) | 2009-06-18 |
KR20040075980A (ko) | 2004-08-30 |
WO2003066919A2 (fr) | 2003-08-14 |
DE03712292T1 (de) | 2005-03-31 |
FR2835533B1 (fr) | 2004-10-08 |
KR100964855B1 (ko) | 2010-06-24 |
AU2003216971A8 (en) | 2003-09-02 |
CA2471501C (fr) | 2010-05-11 |
ATE413476T1 (de) | 2008-11-15 |
US20050028894A1 (en) | 2005-02-10 |
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