WO2004090183A1 - High strength al-zn alloy and method for producing such an alloy product - Google Patents

High strength al-zn alloy and method for producing such an alloy product Download PDF

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Publication number
WO2004090183A1
WO2004090183A1 PCT/EP2004/003997 EP2004003997W WO2004090183A1 WO 2004090183 A1 WO2004090183 A1 WO 2004090183A1 EP 2004003997 W EP2004003997 W EP 2004003997W WO 2004090183 A1 WO2004090183 A1 WO 2004090183A1
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Prior art keywords
alloy
product
alloy according
range
weight
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PCT/EP2004/003997
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English (en)
French (fr)
Inventor
Rinze Benedictus
Christian Joachim Keidel
Alfred Ludwig Heinz
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Novelis Koblenz GmbH
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Corus Aluminium Walzprodukte GmbH
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Application filed by Corus Aluminium Walzprodukte GmbH filed Critical Corus Aluminium Walzprodukte GmbH
Priority to BRPI0409360-7A priority Critical patent/BRPI0409360A/pt
Priority to CA2519387A priority patent/CA2519387C/en
Priority to DE112004000596T priority patent/DE112004000596B4/de
Priority to AT0911004A priority patent/AT502294B1/de
Priority to GB0520502A priority patent/GB2415203B/en
Priority to JP2006505139A priority patent/JP4964586B2/ja
Priority to CN200480009567.XA priority patent/CN1780925B/zh
Publication of WO2004090183A1 publication Critical patent/WO2004090183A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C22C21/10—Alloys based on aluminium with zinc 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
    • C22F1/053—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 zinc as the next major constituent

Definitions

  • the present invention relates to a wrought high strength Al-Zn alloy with an improved combination of corrosion resistance and toughness according to claim 1, a method for producing a wrought high strength Al-Zn alloy with an improved combination of corrosion resistance and toughness according to claim 9 and a plate product of such alloy, optionally produced in accordance with the method. More specifically, the present invention relates to a wrought high strength Al-Zn alloy designated by the 7000-series of the international nomenclature of the Aluminium Association for structural aeronautical applications. Even more specifically, the present invention relates to a new chemistry window for an Al-Zn alloy having improved combinations of strength, toughness and corrosion resistance, which does not need specific ageing or temper treatments.
  • Aluminium alloys AA7050 and AA7150 exhibit high strength in T6-type tempers, see e.g. US-6,315,842. Also precipitation-hardened AA7x75, AA7x55 alloy products exhibit high strength values in the T6 temper.
  • the T6 temper is known to enhance the strength of the alloy, wherein the aforementioned AA7x50, AA7x75 and AA7x55 alloy products which contain high amounts of zinc, copper and magnesium are known for their high strength-to-weight ratios and, therefore, find application in particular in the aircraft industry.
  • these applications result in exposure to a wide variety of climatic conditions necessitating careful control of working and ageing conditions to provide adequate strength and resistance to corrosion, including both stress corrosion and exfoliation.
  • T74 temper is a limited over-aged condition, between T73 and T76, in order to obtain an acceptable level of tensile strength, stress corrosion resistance, exfoliation corrosion resistance and fracture toughness.
  • T74 temper is performed by over-ageing the aluminium alloy product at temperatures of 121 °C for 6 to 24 hours and 171 °C for about 14 hours.
  • EP-0377779 discloses an improved process for producing a 7055 alloy for sheet or thin plate applications in the field of aerospace such as upper-wing members with high toughness and good corrosion properties which comprises the steps of working a body having a composition consisting of, in wt.%: Zn: 7.6 - 8.4 Cu: 2.2 - 2.6 Mg: 1.8 - 2.1 , one or more elements selected from Zr: 0.5 - 0.2
  • Hf 0.03 - 0.5, the total of said elements not exceeding 0.6 wt.%, the balance aluminium plus incidental impurities, solution heat treating and quenching said product and artificially ageing the product by either heating the product three times in a row to one or more temperatures from 79°C to 163°C or heating such product first to one or more temperatures from 79°C to 141 °C for two hours or more or heating the product to one or more temperatures from 148°C to 174°C.
  • These products show an improved exfoliation corrosion resistance of "EB" or better with about 15% greater yield strength than similar sized AA7x50 counter- parts in the T76-temper condition.
  • US-5,312,498 discloses another method for producing an aluminium-based alloy product having improved exfoliation resistance and fracture toughness with balanced zinc, copper and magnesium levels such that there is no excess of copper and magnesium.
  • the method of producing the aluminium-based alloy product utilizes either a one- or two-step ageing process in conjunction with the stochiometrically balancing of copper, magnesium and zinc. A two-step ageing sequence is disclosed wherein the alloy is first aged at approx.
  • Such ageing method is directed to thin plate or sheet products, which are used for lower-wing, skin applications or fuselage skin.
  • US-4,954,188 discloses a method for providing a high strength aluminium alloy characterised by improved resistance to exfoliation using an alloy consisting of the following alloying elements, in wt.%: Zn: 5.9 - 8.2 Cu: 1.5 - 3.0 Mg: 1.5 - 4.0 Cr: ⁇ 0.04, other elements such as zirconium, manganese, iron, silicon and titanium in total less than 0.5, the balance aluminium, working the alloy into a product of a predetermined shape, solution heat treating the reshaped product, quenching, and ageing the heat treated and quenched product to a temperature of from 132°C to 140°C for a period of from 6 to 30 hours.
  • the desired properties of having high strength, high toughness and high corrosion resistance were achieved in this alloy by lowering the ageing temperature rather than raising the temperature as taught previously from e.g. US-3,881 ,966 or US-3,794,531.
  • US-5,221 ,377 therefore discloses an alloy product consisting essentially of about 7.6 to 8.4 wt.% Zn, about 1.8 to 2.2 wt.% Mg and about 2.0 to 2.6 wt.% Cu.
  • Such alloy product exhibits a yield strength, which is about 10 % greater than its
  • US-5,496,426 discloses an alloy as disclosed in US-5,221 ,377 and a process including hot rolling, annealing and cold rolling within a preferred cold reduction range of 20 % to 70 % which, in turn, is preferably followed by controlled annealing thereby displaying characteristics which are better than AA7075-T6 characteristics.
  • US-5, 108,520 and US-4,477,292 disclose an ageing process for solution- heat-treated, precipitation hardening metal alloy including three steps of ageing, comprising (1) ageing the alloy at one or more temperatures substantially above room temperature but below 163°C to substantially below peak yield strength, (2) subsequently ageing the alloy at one or more temperatures at about 190°C for increasing the resistance of the alloy to corrosion and thereafter, (3) ageing the alloy at one or more temperatures substantially above room temperature but below about 163°C for increasing yield strength.
  • the resultant product displayed good strength- properties and a good corrosion performance.
  • the three step ageing procedure is cumbersome and difficult to perform so that the costs for producing such alloy increase.
  • the present invention has a number of preferred objects.
  • the above objects of the invention are achieved by using the characterizing features of claim 1. Further preferred embodiments are described and specified within the sub-claims.
  • a preferred method to produce such alloy is defined in claim 9 and a respective plate product is claimed and described in claim 14 and corresponding sub-claims.
  • alloy designations and temper designations refer to the Aluminum Association designations in Aluminum Standards and Data and the Registration Records, all published by the US Aluminum Association. All percentages are in weight percents, unless otherwise indicated.
  • the above mentioned objects of the invention are achieved by using a high strength Al-Zn alloy product with an improved combination of corrosion resistance and toughness, the alloy comprising essentially (in wt.%):
  • Such chemistry window for an AA7000-series alloy exhibits excellent properties when produced to thin plate products which is preferably useable in aerospace upper-wing applications.
  • the above-defined chemistry has properties, which are comparable or better than existing alloys of the AA7x50 or AA7x55 series in the T77-temper, without using the above-described cumbersome and complicated T77 ageing cycles.
  • the chemistry leads to an aluminium product which is not only superior with regard to the question of costs but also simpler to produce since less processing steps are necessary. Additionally, the chemistry allows new manufacturing techniques like age creep forming which is not feasible when a T77-temper alloy is applied. Even better, the chemistry as defined above can also be aged to the T77-temper wherein the corrosion resistance further improves as compared to the two-step ageing procedure, which is described herein below, wherein especially the exfoliation corrosion performance is enhanced.
  • a preferred amount of magnesium is in a range of 0.2[Cu] + 1.3 ⁇ [Mg] ⁇ 0.1 [Cu] + 2.15, most preferably in a range of 0.2[Cu] + 1.4 ⁇ [Mg] ⁇ 0.1 [Cu] + 1.9.
  • Copper is in a range of about 1.5 to 2.1 , more preferably in a range of 1.5 to less than 2.0. The balance of magnesium and copper is important for the inventive chemistry.
  • Copper and magnesium are important elements for adding strength to the alloy. Too low amounts of magnesium and copper result in a decrease of strength while too high amounts of magnesium and copper result in a lower corrosion performance and problems with the weldability of the alloy product.
  • Prior art techniques used special ageing procedures to ameliorate the strength and low amounts of magnesium and copper are used in order to achieve a good corrosion performance.
  • toughness and corrosion performance copper and magnesium amounts (in wt.%) of between about 1.5 and 2.3 have been found to give a good balance for thick alloy products.
  • the corrosion performance is the vital parameter for thin alloy products so that less amounts of copper and magnesium must be used, thereby resulting in a lower strength.
  • the claimed chemistry of the present invention it is now possible to achieve strength levels in the region of a T6-temper alloy while maintaining corrosion performance characteristics similar to those of T74-temper alloys.
  • the improved corrosion resistance of the alloy according to the invention has exfoliation resistance properties ("EXCO") of EB or better, preferably EA or better.
  • T73, T74 and T76 along with typical performance of T6, tempers.
  • SCC standards To determine whether commercial alloys meet the SCC standards, a given test specimen is subjected to predefined test conditions. Bar-shaped specimens are exposed to cycles of immersing in a 3.5% NaCI aqueous solution for 10 minutes, followed by
  • Stress level Such testing is usually carried out for a minimum of 20 days (or for less time should the specimen fail or crack before 20 days have passed). This test is the ASTM standard G47 (G47-98) test.
  • G47 (G38-73) is used for extruded alloy products that include thin plate products.
  • This test consists of compressing the opposite ends of a C-shaped ring using constant strain levels and alternate immersion conditions substantially similar to those as described above. While an AA7075, AA7050 or AA7150-T6 tempered alloy fails the SCC test in less than 20 days and while the exfoliation properties are
  • T73 The exfoliation properties of T73 are EA or better. Specific examples are described herein below.
  • the inventive alloy has a chemistry with a preferred amount of magnesium and copper of about 1.93 when the amount (in wt.%) of zinc is about 8.1. However, the amount (in wt.%) of zinc is in a range of 6.1 to 8.3, more preferably in a range of 6.1 to 7.0 if manganese is lower than 0.05, and preferably lower than 0.02. Some preferred embodiments of the present invention are described within the examples herein below.
  • the amount of manganese (in wt.%) is preferably in a range of about 0.06 to
  • Manganese contributes to or aids in grain size control during operations that can cause the alloy microstructure to recrystallize.
  • the preferred levels of manganese are lower than in conventional AA7000-series alloys but may be raised when zinc is raised.
  • the amount of the additional alloying elements Ce and/or Sc is smaller than
  • 0.20 preferably in a range of 0.05 to 0.15, most preferably around 0.10.
  • a preferred method for producing a wrought high strength Al-Zn alloy product with an improved combination of corrosion resistance and toughness comprises the steps of a) casting an ingot with the following composition (in weight percent):
  • the properties of the invention may be further achieved throughout a preferred method which includes artificially ageing the worked and solution heat- treated product, wherein the ageing step comprises a first heat treatment at a temperature in a range of 105°C to 135°C, preferably around 120°C for 2 to 20 hours, preferably around 8 hours, and a second heat treatment at a higher temperature than 135°C but below 210°C, preferably around 155°C for 4 to 12 hours, preferably 8 to 10 hours.
  • a corrosion performance is achieved which is similar to the corrosion performance of a T76-temper alloy.
  • the ageing step comprises a third heat treatment at a temperature in a range of 105°C to 135°C for more than 20 hours and less than 30 hours.
  • This T77-temper ageing procedure is known and even increases the performance characteristics as compared to the two-step ageing procedure.
  • the two- step ageing procedure results in thin aluminium alloy products, which are partially comparable and partially better than T77-temper products.
  • Such plate product of high strength Al-Zn alloy may be obtained by an alloy having a composition as described above or being produced in accordance with a method as described above.
  • Such plate product is preferably useable as thin aircraft member, more preferably as an elongated structural shape member. Even more preferred is a plate product for use as an upper-wing member, preferably a thin skin member of an upper-wing or of a stringer of an aircraft.
  • Tests were performed comparing the performance of the alloy according to the present invention and AA7150-T77 alloys. It has been found that the examples of the alloy of the present invention show an improvement over conventional AA7150-T77-temper alloys.
  • alloys 1 , 2 and 4 show better strength/toughness combinations. Alloys 2, 3 and 4 all have an acceptable EXCO performance wherein alloys 2, 3 and 4 have a significant higher compression yield strength than alloy No. 1 (AA7050-alloy). Alloys 2 and 4 exhibit a property balance that makes them very suitable for upper-wing applications in aerospace thereby showing a balance of properties, which is better than those of conventional 7150- T77 alloys. However, it is still possible to use a T77-temper for the inventive alloys as shown in Table 3.
  • AA7055-T77 alloys are preferred instead of AA7150-T77 alloys as an alloy for upper wing applications.
  • the present invention therefore discloses optimised copper and magnesium windows, which show properties equal or better than conventional AA7055-T77 alloys.
  • alloys 3 to 8 and 11 displayed good toughness properties
  • alloys 1 to 5 and 9 and 10 displayed good strength properties.
  • alloys 3, 4 and 5 show a good balance of strength and toughness so that it is clear to have a copper content of above 1.3 and a magnesium content of above 1.6 (in wt.%) when zinc is present in an amount of 8.1. Such amounts are lower limits for the copper and magnesium windows.
  • Table 6 the toughness will drop to un-acceptable low-levels when copper and magnesium levels are too high (alloys 1, 2, 9 and 10).
  • AA7055-T77 alloys are preferred instead of AA7150-T77 alloys as an alloy for upper wing applications.
  • the present invention therefore discloses optimised copper and magnesium windows, which show properties equal or better to conventional AA7055-T77 alloys.
  • Alloys 1 and 2 were tested with regard to their strength properties. These properties are shown in Table 10. Alloy 2 has been tempered in accordance with two temper conditions (T79-T76 and T77). Reference alloy AA7055 has been measured in T77 temper (M-Ref) while the technical data of an AA7055 reference alloy in a T77 temper are given as well (as identified by Ref).
  • the inventive alloy has similar tensile properties as a conventional AA7055- T77 alloy. However, the properties in the ST direction are better than those of the conventional AA7055-T77 alloy. Also the stress corrosion performance is better than of an AA055-T77 alloy.
  • the inventive alloy can therefore be used as an inexpensive substitute for AA7055-T77 tempered alloys which is also useable for age-creep forming, thereby showing a superior compression yield strength and corrosion resistance.

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PCT/EP2004/003997 2003-04-10 2004-04-09 High strength al-zn alloy and method for producing such an alloy product Ceased WO2004090183A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
BRPI0409360-7A BRPI0409360A (pt) 2003-04-10 2004-04-09 liga de al-zn de alta resistência e método para produzir um produto de tal liga
CA2519387A CA2519387C (en) 2003-04-10 2004-04-09 High strength al-zn alloy and method for producing such an alloy product
DE112004000596T DE112004000596B4 (de) 2003-04-10 2004-04-09 Hochfeste Al-Zn-Legierung und Verfahren zum Herstellen eines solchen Legierungsprodukts
AT0911004A AT502294B1 (de) 2003-04-10 2004-04-09 Al-zn-knetlegierung und verwendung einer solchen legierung
GB0520502A GB2415203B (en) 2003-04-10 2004-04-09 High strength Al-Zn alloy and method for producing such an alloy product
JP2006505139A JP4964586B2 (ja) 2003-04-10 2004-04-09 高強度Ａｌ−Ｚｎ合金およびそのような合金製品の製造方法
CN200480009567.XA CN1780925B (zh) 2003-04-10 2004-04-09 高强度Al-Zn合金和这种合金产品的生产方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP03076049.0 2003-04-10
EP03076049 2003-04-10

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WO2004090183A1 true WO2004090183A1 (en) 2004-10-21

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US (2) US20050034794A1 (enExample)
JP (1) JP4964586B2 (enExample)
CN (2) CN103146969B (enExample)
AT (1) AT502294B1 (enExample)
BR (1) BRPI0409360A (enExample)
CA (2) CA2519387C (enExample)
DE (1) DE112004000596B4 (enExample)
ES (2) ES2398002B2 (enExample)
FR (1) FR2853666B1 (enExample)
GB (1) GB2415203B (enExample)
RU (1) RU2353699C2 (enExample)
WO (1) WO2004090183A1 (enExample)

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GB2415202B (en) * 2003-04-10 2007-08-29 Corus Aluminium Walzprod Gmbh An Al-Zn-Mg-Cu alloy
CN100441715C (zh) * 2005-03-07 2008-12-10 东北轻合金有限责任公司 铝合金自由锻件及其制造方法
WO2009156283A1 (en) * 2008-06-24 2009-12-30 Aleris Aluminum Koblenz Gmbh Al-zn-mg alloy product with reduced quench sensitivity
US8088234B2 (en) 2006-07-07 2012-01-03 Aleris Aluminum Koblenz Gmbh AA2000-series aluminum alloy products and a method of manufacturing thereof
CN102760508A (zh) * 2012-07-18 2012-10-31 中南大学 含Hf和Ce的高电导率抗蠕变铝合金电缆导体及制备方法
US8608876B2 (en) 2006-07-07 2013-12-17 Aleris Aluminum Koblenz Gmbh AA7000-series aluminum alloy products and a method of manufacturing thereof
US9353430B2 (en) 2005-10-28 2016-05-31 Shipston Aluminum Technologies (Michigan), Inc. Lightweight, crash-sensitive automotive component
CN106399775A (zh) * 2016-11-11 2017-02-15 湖北万佳宏铝业股份有限公司 一种高强度铝合金材料配方及其制备方法
EP1902150B1 (en) 2005-03-24 2018-06-20 Kaiser Aluminum Fabricated Products, LLC High strength aluminum alloys and process for making the same
WO2019007817A1 (en) 2017-07-03 2019-01-10 Constellium Issoire AL-ZN-CU-MG ALLOYS AND PROCESS FOR PRODUCING THE SAME
WO2019063490A1 (en) 2017-09-26 2019-04-04 Constellium Issoire HIGH RESISTANCE AL-ZN-CU-MG ALLOYS AND METHOD OF MANUFACTURE
EP3670690A1 (en) 2018-12-20 2020-06-24 Constellium Issoire Al-zn-cu-mg alloys and their manufacturing process
US11421309B2 (en) 2015-10-30 2022-08-23 Novelis Inc. High strength 7xxx aluminum alloys and methods of making the same
EP3987072A4 (en) * 2019-06-24 2023-07-19 Arconic Technologies LLC ADVANCED THICK WROUGHT 7XXX ALUMINUM ALLOYS AND PROCESSES THEREOF
EP4386097A1 (en) 2022-12-12 2024-06-19 Constellium Rolled Products Ravenswood, LLC 7xxx wrought products with improved compromise of tensile and toughness properties and method for producing
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US7883591B2 (en) * 2004-10-05 2011-02-08 Aleris Aluminum Koblenz Gmbh High-strength, high toughness Al-Zn alloy product and method for producing such product
DE502005001724D1 (de) 2005-01-19 2007-11-29 Fuchs Kg Otto Abschreckunempfindliche Aluminiumlegierung sowie Verfahren zum Herstellen eines Halbzeuges aus dieser Legierung
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US8157932B2 (en) * 2005-05-25 2012-04-17 Alcoa Inc. Al-Zn-Mg-Cu-Sc high strength alloy for aerospace and automotive castings
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US8673209B2 (en) * 2007-05-14 2014-03-18 Alcoa Inc. Aluminum alloy products having improved property combinations and method for artificially aging same
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US8206517B1 (en) 2009-01-20 2012-06-26 Alcoa Inc. Aluminum alloys having improved ballistics and armor protection performance
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CN102978544B (zh) * 2012-11-21 2014-08-20 中南大学 一种Al-Zn-Mg-Cu系铝合金板材多级蠕变时效成形方法
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GB2415202B (en) * 2003-04-10 2007-08-29 Corus Aluminium Walzprod Gmbh An Al-Zn-Mg-Cu alloy
US10472707B2 (en) 2003-04-10 2019-11-12 Aleris Rolled Products Germany Gmbh Al—Zn—Mg—Cu alloy with improved damage tolerance-strength combination properties
CN100441715C (zh) * 2005-03-07 2008-12-10 东北轻合金有限责任公司 铝合金自由锻件及其制造方法
EP1902150B1 (en) 2005-03-24 2018-06-20 Kaiser Aluminum Fabricated Products, LLC High strength aluminum alloys and process for making the same
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RU2443797C2 (ru) * 2006-07-07 2012-02-27 Алерис Алюминум Кобленц Гмбх Продукты из алюминиевого сплава серии аа7000 и способ их изготовления
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WO2009156283A1 (en) * 2008-06-24 2009-12-30 Aleris Aluminum Koblenz Gmbh Al-zn-mg alloy product with reduced quench sensitivity
US9890448B2 (en) 2008-06-24 2018-02-13 Aleris Aluminum Koblenz Gmbh Al—Zn—Mg alloy product with reduced quench sensitivity
CN102760508A (zh) * 2012-07-18 2012-10-31 中南大学 含Hf和Ce的高电导率抗蠕变铝合金电缆导体及制备方法
US11421309B2 (en) 2015-10-30 2022-08-23 Novelis Inc. High strength 7xxx aluminum alloys and methods of making the same
CN106399775A (zh) * 2016-11-11 2017-02-15 湖北万佳宏铝业股份有限公司 一种高强度铝合金材料配方及其制备方法
WO2019007817A1 (en) 2017-07-03 2019-01-10 Constellium Issoire AL-ZN-CU-MG ALLOYS AND PROCESS FOR PRODUCING THE SAME
WO2019063490A1 (en) 2017-09-26 2019-04-04 Constellium Issoire HIGH RESISTANCE AL-ZN-CU-MG ALLOYS AND METHOD OF MANUFACTURE
EP3688202B1 (en) 2017-09-26 2023-01-18 Constellium Issoire Al- zn-cu-mg alloys with high strength and method of fabrication
US12421578B2 (en) 2017-09-26 2025-09-23 Constellium Issoire Al—Zn—Cu—Mg alloys with high strength and method of fabrication
EP3670690A1 (en) 2018-12-20 2020-06-24 Constellium Issoire Al-zn-cu-mg alloys and their manufacturing process
WO2020127592A1 (en) 2018-12-20 2020-06-25 Constellium Issoire Al- zn-cu-mg alloys and their manufacturing process
EP3987072A4 (en) * 2019-06-24 2023-07-19 Arconic Technologies LLC ADVANCED THICK WROUGHT 7XXX ALUMINUM ALLOYS AND PROCESSES THEREOF
EP4386097A1 (en) 2022-12-12 2024-06-19 Constellium Rolled Products Ravenswood, LLC 7xxx wrought products with improved compromise of tensile and toughness properties and method for producing
WO2024126341A1 (en) 2022-12-12 2024-06-20 Constellium Rolled Products Ravenswood, Llc 7xxx wrought products with improved compromise of tensile and toughness properties and method for producing

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US20050034794A1 (en) 2005-02-17
CA2519387C (en) 2015-06-02
AT502294A1 (de) 2007-02-15
ES2398002B2 (es) 2015-01-22
CA2881183A1 (en) 2004-10-21
ES2398002A1 (es) 2013-03-13
DE112004000596T5 (de) 2006-03-09
AT502294B1 (de) 2010-02-15
CN103146969A (zh) 2013-06-12
RU2005134846A (ru) 2006-04-10
GB2415203B (en) 2007-01-03
CA2881183C (en) 2018-06-12
FR2853666B1 (fr) 2007-05-11
ES2288389A1 (es) 2008-01-01
DE112004000596B4 (de) 2011-03-24
CN103146969B (zh) 2015-07-08
FR2853666A1 (fr) 2004-10-15
GB0520502D0 (en) 2005-11-16
CN1780925A (zh) 2006-05-31
JP4964586B2 (ja) 2012-07-04
BRPI0409360A (pt) 2006-04-25
JP2006522872A (ja) 2006-10-05
RU2353699C2 (ru) 2009-04-27
CN1780925B (zh) 2013-03-27
GB2415203A (en) 2005-12-21

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