WO2006011242A1 - Aluminum alloy sheet and method for manufacturing the same - Google Patents
Aluminum alloy sheet and method for manufacturing the same Download PDFInfo
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- WO2006011242A1 WO2006011242A1 PCT/JP2004/011323 JP2004011323W WO2006011242A1 WO 2006011242 A1 WO2006011242 A1 WO 2006011242A1 JP 2004011323 W JP2004011323 W JP 2004011323W WO 2006011242 A1 WO2006011242 A1 WO 2006011242A1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
- B22D11/003—Aluminium alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0605—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by two belts, e.g. Hazelett-process
-
- 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
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
-
- 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
- C22F1/047—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 magnesium as the next major constituent
Definitions
- the present invention relates to an aluminum alloy sheet and a method for manufacturing the same, and in particular, it relates to an aluminum alloy sheet which is a forming material suitable for automobile body sheets and the like.
- Body panels of automobiles have been primarily made from cold-rolled steel sheets until now.
- the use of aluminum alloy sheets of Al-Mg base, Al-Mg-Si base, and the like has been studied recently.
- Generally known methods for manufacturing these aluminum alloy sheets includes a method in which a slab is cast by a DC casting method (semi-continuous casting), the slab is subjected to scalping and the resulting slab is inserted into a batch type furnace and is subjected to a homogenization treatment (soaking) for a few hours to about ten hours, followed by a hot rolling step, a cold rolling step, and an annealing step, so that a sheet having a predetermined thickness is completed (refer to, for example, JPP3155678) .
- a twin belt casting method in which a pair of parallel-opposed rotating endless belts are disposed, a melt of aluminum alloy is introduced into the gap between these endless belts, and is continuously taken out while being cooled, followed by being rewound around a coil (refer to, for example, PCT WO 2002/011922 (JP2004- 505774A)).
- intermetallic compounds e.g., Al-(Fe 1 Mn)-Si
- crystallized in the matrix may grow to have size of ten to several tens of micrometers, particularly in the central portion of the slab.
- Such a intermetallic compound may adversely affect the press formability of a final annealed sheet prepared through a rolling and annealing step. That is, when the final annealed sheet is deformed, if the size of the intermetallic compounds is relatively large, peeling (so-called void) tends to occur between the intermetallic compound and the matrix.
- microcracks starting from this peeled portion may occur, so that the press formability may be deteriorated.
- dislocations accumulate around the intermetallic compound during cold rolling, and these dislocations serve nucleation sites for re ⁇ rystallization during annealing. Therefore, if the intermetallic compounds become large, the number of intermetallic compounds per unit volume is decreased and, thereby, the concentration of nucleation sites for recrystallization grains is decreased. Consequently, the recrystallized grain size increases several tens of micrometers, and the press formability is deteriorated.
- a high Mg alloy is adopted to improve the press formability. However, if the content of Mg is increased, ⁇ phases precipitates in the shape of a film at grain boundaries as time goes by after the press forming is performed and, thereby, the stress corrosion cracking resistance is deteriorated.
- steps e.g., scalping of the slab surface after the DC casting, a homogenization treatment, hot rolling, cold rolling, and intermediate annealing
- steps e.g., scalping of the slab surface after the DC casting, a homogenization treatment, hot rolling, cold rolling, and intermediate annealing
- the belt casting method the slab prepared by continuous casting of a melt is subjected to cold rolling and, therefore, there are advantages in that the steps are simplified compared with those in the DC casting method, and the manufacturing cost can be reduced.
- no study has been conducted with respect to the improvement of quality, e.g., the press formability and the stress corrosion cracking resistance of the final annealed sheet.
- an aluminum alloy slab ingot used in the present invention is prepared by casting a melt containing 3.3 to 3.6 percent by weight of Mg and 0.1 to 0.2 percent by weight of Mn, furthermore, 0.05 to 0.3 percent by weight of Fe and 0.05 to 0.15 percent by weight of Si, and the remainder comprised of Al and incidental impurities into a slab of 5 to 15 mm in thickness with a twin belt type caster in order that the region of one quarter-thickness below the surface is cooled at a cooling rate of 20°C/sec to 200°C/sec.
- the resulting aluminum alloy slab ingot is directly rewinded around a roll, the slab ingot is cold-rolled with a rolling roll having a surface roughness of Ra 0.2 to 0.8 ⁇ m and, thereafter, annealing is performed in order that the size of intermetallic compounds becomes 5 ⁇ m or less, the recrystallized grain size becomes 15 ⁇ m or less in the region at a depth of 10 to 30 ⁇ m below the sheet surface of the final annealed sheet, and the surface roughness becomes Ra 0.2 to 0.7 ⁇ m. Consequently, an aluminum alloy sheet having excellent press formability and stress corrosion cracking resistance can be prepared.
- a melt is introduced into a twin belt type caster, a slab is continuously cast, and the resulting slab is rewinded around a roll.
- a twin belt type caster for example, a pair of parallel-opposed rotating endless belts are disposed, the melt is introduced into a flat portion sandwiched between the belts, and is transferred in accordance with the rotation of the belts, so that the melt is cooled and, thereby, a slab having a predetermined sheet thickness is cast continuously.
- the slab cast with the twin belt type caster has a total thickness of, for example, 5 to 15 mm, and a region of one quarter-thickness below the surface relative to the total slab thickness is cooled at a cooling rate of 20° C/sec to 200° C/sec during the casting. Consequently, the size of intermetallic compounds of Al-(Fe-Mn)-Si base and the like becomes a very fine 5 ⁇ m or less in the region at a depth of 10 to 30 ⁇ m below the sheet surface of the final annealed sheet.
- dislocations accumulate around the intermetallic compounds during cold rolling, and these dislocations serve as nucleation sites for recrystallization.
- the number of intermetallic compounds per unit volume is increased and, thereby, the concentration of nucleation sites for recrystallization is increased. Consequently, the recrystallized grain size becomes relatively small 15 ⁇ m or less, and a final annealed sheet having excellent press formability can be produced.
- the surface roughness of the roll is controlled at within the range of Ra 0.2 to 0.8 ⁇ m in the present embodiment.
- the shape of the rolling-roll surface is transferred to the rolled sheet surface during the cold- rolling step and, thereby, the surface roughness of the final annealed sheet becomes Ra 0.2 ⁇ m to 0.7 ⁇ m.
- the surface shape of the final annealed sheet serves the function as micropools to uniformly hold low-viscosity lubricant used during the forming and, thereby, a predetermined press formability can be ensured.
- the strength of the final annealed sheet is increased and, in addition, the work hardenability is enhanced to increase the ductility, so that an improvement of the press formability is accelerated.
- the amount of addition is specified as being 3.3 to 3.6 percent by weight because if less than 3.3 percent by weight, the strength is low and the formability is poor, and if more than 3.6 percent by weight, the stress corrosion cracking resistance (SCC resistance) is deteriorated and the manufacturing cost is increased.
- the amount of addition is specified as being 0.1 to 0.2 percent by weight because if less than 0.1 percent by weight, the effect thereof is not adequately exhibited, and if more than 0.2 percent by weight, intermetallic compounds of Al-(Fe-Mn)-Si base are increased and, thereby, the ductility of the material is decreased, so that the formability of an aluminum sheet for an automobile is deteriorated.
- the content of Fe is preferably within the range of 0.05 to 0.3 percent by weight, and more preferably is 0.05 to 0.2 percent by weight.
- the content of Si is preferably within the range of 0.05 to 0.15 percent by weight, and more preferably is 0.05 to 0.10 percent by weight.
- the size of intermetallic compounds in the region at a depth of 10 to 30 ⁇ m below the sheet surface of the final annealed sheet is 5 ⁇ m or less.
- the size of the intermetallic compounds is 5 ⁇ m or less, peeling is difficult to occur between the intermetallic compounds and the matrix, occurrence of microcracks starting from the peeled portion is suppressed, and the press formability are improved.
- the size of the intermetallic compounds is 5 ⁇ m or less, the number of intermetallic compounds per unit volume is increased and, thereby, the concentration of nucleation sites for recrystallization is increased during the annealing. Consequently, the size of recrystallized grains becomes a relatively small 15 ⁇ m or less, and the effect of improving the press formability is exhibited.
- the size of recrystallized grains in the sheet surface layer of the final annealed sheet is 15 ⁇ m or less. If the size exceeds 15 ⁇ m not only formability is deteriorated, height differences generated at grain boundaries during deformation of the material become too large, orange peel after deformation becomes remarkable and, thereby, deterioration of the quality of the surface after the press forming is brought about.
- the surface roughness of the final annealed sheet is Ra 0.2 to 0.7 ⁇ m. If the surface roughness is less than Ra 0.2 ⁇ m, generation of micropools to hold low- viscosity lubricant used during the forming on the final annealed sheet becomes inadequate and, thereby, it becomes difficult to uniformly penetrate the lubricant into the interface between the sheet surface and the press dies, so that the press formability is not improved. On the other hand, if the surface roughness exceeds Ra 0.7 ⁇ m, micropools are sparsely and nonuniformly distributed on the final annealed sheet and, thereby, it becomes difficult to uniformly hold the lubricant on the sheet surface, so that - li ⁇
- the surface roughness of the final annealed, sheet is more preferably Ra 0.3 to 0.6 ⁇ m.
- the alloy component may contain 0.10 percent by weight or less of grain refiner for cast slab (for example, Ti) . Furthermore, the alloy component may contain Cu, V, Zr, and the like as impurities at a content within the range of 0.05 percent by weight or less each.
- the thickness of the slab prepared with a twin belt type caster is specified as being within the range of 5 to 15 mm because if the thickness is less than 5 mm, the amount of melt passing through the caster on a unit time basis is small and, therefore, it becomes difficult to perform the casting, and if the thickness exceeds 15 mm, rewinding with a roll becomes impossible.
- the slab With respect to the slab prepared by DC casting, the slab has a large thickness, and in the metal structure, intermetallic compounds, e.g., Al-(Fe*Mn)-Si, crystallized in the central portion of the slab may have size reaching ten to several tens of micrometers because the cooling rate is a relatively low one to ten-odd degrees centigrade per second. In this case, peeling may occur between the intermetallic compounds and the matrix during plastic deformation so as to adversely affect the press formability.
- intermetallic compounds e.g., Al-(Fe*Mn)-Si
- the slab can be controlled to have a reduced thickness
- the cooling rate of the region of one quarter-sheet thickness below the surface can be increased to 20° C/sec to 200°C/sec and, thereby, the size of intermetallic compounds in the region at a depth of 10 to 30 ⁇ m below the sheet surface of the final annealed sheet is allowed to become 5 ⁇ m or less.
- the surface roughness of the roll surface is specified as being Ra 0.2 to 0.8 ⁇ m to control the surface roughness of the final annealed sheet.
- the surface roughness of the final annealed sheet becomes Ra 0.2 to 0.7 ⁇ m.
- the surface shape of the final annealed sheet serves the function as micropools to uniformly hold the low- viscosity lubricant used during the forming and, thereby, a sheet having excellent press formability can be provided.
- the surface roughness of the final annealed sheet is more preferably Ra 0.3 to 0.6 ⁇ m
- the surface roughness of the cold rolling roll is more preferably specified as being Ra 0.3 to 0.7 ⁇ m.
- an aluminum alloy sheet having excellent press formability and stress corrosion cracking resistance in particular, an aluminum alloy sheet suitable for the use in an automobile can be provided.
- a melt having a composition A shown in Table 1 was degassed and settled, and subsequently, a slab was cast by a twin belt caster. The resulting slab was cold-rolled into a sheet of 1 mm in thickness with a cold-rolling roll. The resulting sheet was continuously annealed (CAL) at 420° C and, thereby, a test specimen of a final annealed sheet was prepared.
- Table 2 (Examples 1 to 3) shows an example of manufacturing condition of the test specimen in each manufacturing process.
- the remainder is composed of Al and incidental impurities,
- the recrystallization grain size, the maximum size of intermetallic compounds, the surface roughness, the 0.2 percent yield strength (0.2% YS), the ultimate tensile strength (UTS), the elongation (EL), the deep drawing height, and the stress corrosion cracking resistance (SCC resistance) life of the resulting test specimen were measured.
- the recrystallization grain size of the test specimen was measured by a intercept method.
- a photograph (200 times) of grains in the test specimen was taken with an polarizing microscope, three lines are drawn in a vertical direction and in a horizontal direction each, the number of grains crossing a line is counted, and an average value of grain sizes determined by dividing the length of the line by the number was taken as the recrystallization grain size of the test specimen.
- the sizes of the intermetallic compounds were measured with an image analyzer (LUZEX) .
- the surface roughness of the test specimen was an average roughness Ra, wherein the measurement was performed with a surface roughness tester in accordance with JIS B0601, the measurement direction was a direction perpendicular to the rolling direction, the measurement region was 4 mm, and the cutoff was 0.8 mm.
- the surface roughness of roll was an average roughness Ra, wherein the measurement was performed with a surface roughness tester in accordance with JIS B0601, the measurement direction was a rolling transverse direction, the measurement region was 4 mm, and the cutoff was 0.8 mm, as in the surface roughness of the test specimen.
- the deep drawing height indicates a critical height of forming at breakage while the following die is used. Punch: 40 mm in diameter, shoulder R: 8 mm, die: 42.5 mm in diameter, shoulder R: 8 mm
- the final annealed sheet was cold-rolled at a cold-rolling reduction of 30 percent, and a sensitization treatment was performed at 120° C for 1 week. Thereafter, stress corresponding to 85 percent of the yield strength was applied, immersion in 3.5 percent salt water was performed continuously, and the time elapsed until crack occurred was measured and taken as the SCC resistance life.
- Test specimens were prepared from melts having compositions shown in Table 1 under the manufacturing conditions shown in Table 2 (Comparative examples 1 to 6). The prepared test specimens were evaluated by performing measurements with respect to the same items as those in Examples 1 to 3, and the measurement results are shown in Table 3 (Comparative examples 1 to 6).
- the Mg content is an appropriate 3.4 percent
- specimen includes fine recrystallized grains and intermetallic compounds
- the surface has an appropriate surface roughness of Ra 0.42 to 0.45 ⁇ m and, therefore, excellent deep drawability and excellent SCC resistance are exhibited.
- a melt is introduced into a twin belt type caster, a slab is continuously cast, and resulting slab is rewinded around a roll.
- the cooling is performed during the casting in order that the region of at least one quarter-thickness below the surface relative to the slab thickness is cooled at a cooling rate of 20°C/sec to 200°C/sec.
- Al-(Fe-Mn)-Si based intermetallic compounds and the like are allowed to become very fine 5 ⁇ m or less. Consequently, peeling between the intermetallic compounds and the matrix is difficult to occur even when the final annealed sheet is deformed, and a sheet having excellent press formability can be produced.
- the recrystallized grain size becomes a relatively small 15 ⁇ m or less and, thereby, a sheet having excellent press formability is provided.
- the surface roughness of the final annealed sheet is allowed to become within the limited range of Ra 0.2 to 0.7 ⁇ m by controlling the surface roughness of the rolling roll at within the range of Ra 0.2 to 0.8 ⁇ m when the roll to be used in the cold rolling is polished with a grinder and, thereby, the surface shape of the final annealed sheet serves the function as micropools to uniformly hold the low-viscosity lubricant used during the forming, so that the press formability can be further improved.
- Comparative example 1 since the Mg content is a low 3.0 percent, all of the ultimate tensile strength, and the elongation are inadequate, and poor deep drawability is exhibited. In Comparative example 2, since the Mg content is a high 4.5 percent, all of the ultimate tensile strength, and the elongation are outstanding, but poor SCC resistance is exhibited.
- the surface roughness Ra is a low 0.1 ⁇ m and, therefore, the surface is smoother than the surfaces in Examples 1 to 3, but poor deep drawability is exhibited.
- the surface roughness Ra is a high 0.8 ⁇ m and, therefore, the surface is rougher than the surfaces in Examples 1 to 3, and poor deep drawability is exhibited in this case as well.
- Comparative example 5 a DC casting material is used. Since the cooling rate during the casting is relatively low. included recrystallized grains and intermetallic compounds are slightly coarser than those in Examples 1 to 3, and poor deep drawability is exhibited. In Comparative example 6, a twin roll casting material is used. Since the cooling rate during the casting is too high, intermetallic compounds are finer than those in Examples 1 to 3, recrystallized grains are coarse, and poor deep drawability is exhibited.
- the resulting aluminum alloy slab cast by a twin belt caster is directly rewound around a roll, the slab is cold-rolled with a rolling roll having a surface roughness of Ra 0.2 to 0.8 ⁇ m and, thereafter, annealing is performed in order that the sizes of intermetallic compounds become 5 ⁇ m or less, the recrystallized grain size becomes 15 ⁇ m or less in the region at a depth of 10 to 30 ⁇ m below the sheet surface of the final annealed sheet, and the surface roughness becomes Ra 0.2 to 0.7 ⁇ m. Consequently, an aluminum alloy sheet having excellent press formability and stress corrosion cracking resistance can be prepared.
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Abstract
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Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2004800437249A CN100469927C (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
US11/572,832 US8425698B2 (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
CA2588046A CA2588046C (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
EP04748272A EP1771590B1 (en) | 2004-07-30 | 2004-07-30 | Method for manufacturing an aluminum alloy sheet |
JP2007503141A JP4740941B2 (en) | 2004-07-30 | 2004-07-30 | Method for producing aluminum alloy plate |
KR1020077004704A KR101057264B1 (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and manufacturing method |
PCT/JP2004/011323 WO2006011242A1 (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2004/011323 WO2006011242A1 (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
Publications (1)
Publication Number | Publication Date |
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WO2006011242A1 true WO2006011242A1 (en) | 2006-02-02 |
Family
ID=34958425
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/011323 WO2006011242A1 (en) | 2004-07-30 | 2004-07-30 | Aluminum alloy sheet and method for manufacturing the same |
Country Status (7)
Country | Link |
---|---|
US (1) | US8425698B2 (en) |
EP (1) | EP1771590B1 (en) |
JP (1) | JP4740941B2 (en) |
KR (1) | KR101057264B1 (en) |
CN (1) | CN100469927C (en) |
CA (1) | CA2588046C (en) |
WO (1) | WO2006011242A1 (en) |
Cited By (7)
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---|---|---|---|---|
EP1794338A2 (en) * | 2004-08-27 | 2007-06-13 | Commonwealth Industries, Inc. | Aluminum automotive structural members |
WO2008078399A1 (en) * | 2006-12-22 | 2008-07-03 | Nippon Light Metal Company, Ltd. | Method of producing aluminum alloy sheet |
JP2008163357A (en) * | 2006-12-26 | 2008-07-17 | Nippon Light Metal Co Ltd | Aluminum alloy sheet for automobile and manufacturing method therefor |
JP2008223054A (en) * | 2007-03-09 | 2008-09-25 | Nippon Light Metal Co Ltd | Aluminum alloy sheet for forming-work having excellent deep drawability and burning/softening resistance, and producing method therefor |
WO2009098732A1 (en) | 2008-02-06 | 2009-08-13 | Nippon Light Metal Co., Ltd. | Aluminum alloy sheet for motor vehicle and process for producing the same |
JP2012107339A (en) * | 2011-12-28 | 2012-06-07 | Nippon Light Metal Co Ltd | Aluminum alloy sheet for automobile and manufacturing method therefor |
CN103946404A (en) * | 2012-03-21 | 2014-07-23 | 日本轻金属株式会社 | Aluminum alloy sheet having excellent press formability and shape fixability, and method for manufacturing same |
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US7377304B2 (en) * | 2005-07-12 | 2008-05-27 | Alcoa Inc. | Method of unidirectional solidification of castings and associated apparatus |
JP2008024964A (en) | 2006-07-18 | 2008-02-07 | Nippon Light Metal Co Ltd | High-strength aluminum alloy sheet and producing method therefor |
US7846554B2 (en) | 2007-04-11 | 2010-12-07 | Alcoa Inc. | Functionally graded metal matrix composite sheet |
US8448690B1 (en) | 2008-05-21 | 2013-05-28 | Alcoa Inc. | Method for producing ingot with variable composition using planar solidification |
US20110130297A1 (en) * | 2009-01-23 | 2011-06-02 | Bae Systems Information And Electronic Systems Integration Inc. | Quantum dot-sensory array for biological recognition |
RU2556171C1 (en) | 2011-07-25 | 2015-07-10 | Ниппон Лайт Метал Компани, Лтд. | Aluminium alloy sheet and its manufacturing method |
CN102912199A (en) * | 2012-10-29 | 2013-02-06 | 虞海香 | Aluminum alloy sheet for vehicle body |
JP6176393B2 (en) * | 2014-04-09 | 2017-08-09 | 日本軽金属株式会社 | High-strength aluminum alloy plate with excellent bending workability and shape freezing property |
CN110475882A (en) * | 2017-04-05 | 2019-11-19 | 诺维尔里斯公司 | With high-intensitive and high formability anodic oxidation quality 5XXX aluminium alloy and preparation method |
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2004
- 2004-07-30 CA CA2588046A patent/CA2588046C/en not_active Expired - Fee Related
- 2004-07-30 JP JP2007503141A patent/JP4740941B2/en not_active Expired - Lifetime
- 2004-07-30 CN CNB2004800437249A patent/CN100469927C/en not_active Expired - Lifetime
- 2004-07-30 KR KR1020077004704A patent/KR101057264B1/en not_active IP Right Cessation
- 2004-07-30 EP EP04748272A patent/EP1771590B1/en not_active Expired - Fee Related
- 2004-07-30 WO PCT/JP2004/011323 patent/WO2006011242A1/en active Application Filing
- 2004-07-30 US US11/572,832 patent/US8425698B2/en active Active
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Also Published As
Publication number | Publication date |
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EP1771590B1 (en) | 2011-09-14 |
US20090007994A1 (en) | 2009-01-08 |
EP1771590A1 (en) | 2007-04-11 |
CA2588046C (en) | 2014-09-30 |
KR101057264B1 (en) | 2011-08-16 |
CA2588046A1 (en) | 2006-02-02 |
CN100469927C (en) | 2009-03-18 |
CN101072888A (en) | 2007-11-14 |
US8425698B2 (en) | 2013-04-23 |
JP4740941B2 (en) | 2011-08-03 |
JP2008508421A (en) | 2008-03-21 |
KR20070049184A (en) | 2007-05-10 |
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