EP2652163B1 - Dicke produkte aus 7xxx-legierungen und deren herstellungsverfahren - Google Patents

Dicke produkte aus 7xxx-legierungen und deren herstellungsverfahren Download PDF

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Publication number
EP2652163B1
EP2652163B1 EP11808242.9A EP11808242A EP2652163B1 EP 2652163 B1 EP2652163 B1 EP 2652163B1 EP 11808242 A EP11808242 A EP 11808242A EP 2652163 B1 EP2652163 B1 EP 2652163B1
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EP
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Prior art keywords
block
hours
temperature
solution
nsr
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EP11808242.9A
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English (en)
French (fr)
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EP2652163A1 (de
Inventor
Cédric GASQUERES
Jean-Etienne Fournier
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Constellium Valais AG
Constellium Issoire SAS
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Constellium Valais AG
Constellium Issoire SAS
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Priority to PL11808242T priority Critical patent/PL2652163T3/pl
Publication of EP2652163A1 publication Critical patent/EP2652163A1/de
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    • 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
    • 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
    • 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

Definitions

  • the present invention generally relates to aluminum alloy products and, more particularly, to such thick 7xxx alloy products, their methods of manufacture and use.
  • Thick aluminum blocks are also useful in the field of mechanical engineering.
  • notch resistance is an important property of use for these products and it can be characterized for example by the NSR, which is the ratio between the elastic limit and the mechanical strength in the presence of a notch (" Sharp-Notch Strength-to-Yield Strength Ratio ") measured according to ASTM-E602.
  • NSR the ratio between the elastic limit and the mechanical strength in the presence of a notch
  • Sharp-Notch Strength-to-Yield Strength Ratio the ratio between the elastic limit and the mechanical strength in the presence of a notch
  • a product is said to be quench sensitive if its static mechanical characteristics, such as its yield strength, decrease as the quenching rate decreases.
  • the quenching rate is the average cooling rate of the product during quenching.
  • the thick blocks should also preferably have low residual stresses. Indeed, the residual stresses cause deformations during the machining which affect the geometry of the mold.
  • the residual stresses can be measured for example by the method described in the patent application WO 2004/053180 .
  • low residual stresses we typically mean a W Tbar value of less than 4 kJ / m 3 , and in general of the order of 2 kJ / m 3
  • the thick blocks must be obtained with a process as fast and economical as possible.
  • the patent EP1587965 discloses an alloy useful for the manufacture of thick blocks, composition (in% by weight) 4.6-5.2% Zn; 2.6-3.0% Mg; 0.1-0.2% Cu; 0.05-0.2% Zr; not more than 0.05% Mn; not more than 0.05% Cr; not more than 0.15% Fe; not more than 0.15% Si; not more than 0.10% Ti and a method of manufacturing these blocks, in which the ingot obtained by continuous casting is used directly as a block.
  • VMRBA The patent application FR 2,341,661 (VMRBA) describes a composition alloy (in% by weight) 4.0-6.2% Zn, 0.8-3.0% Mg, 0-1.5% Cu, 0.05 - 0.30% Zr, 0 - 0.20% Fe, 0-0.15% Si, 0-0.25% Mn, 0-0.10% Ti intended to be forged or kneaded by hot deformation and to be used for construction vehicles, machinery, equipment tanks and tools.
  • the patent application JP81144031 discloses an alloy composition (in% by weight) 4.0-6.5% Zn, 0.4-1.8% Mg, 0.1-0.5% Cu, 0.1-0.5% Zr, and additionally 0.05-0.20% Mn and / or 0.05-0.20% Cr, for the production of tubes.
  • the problem solved by the present invention is to obtain thick aluminum blocks having an improved property compromise between the static mechanical characteristics and the notch resistance, having a low level of residual stresses, by a rapid process. and economic.
  • Yet another object of the invention is the use of a thick block according to the invention for the manufacture of mold for injection of plastics.
  • Figure 1 Compromise obtained between the elastic limit R P.0,2 and the parameter called NSR ("Sharp-Notch Strength-to-Yield Strength Ratio"), which is the ratio of the notched specimen mechanical strength and the elastic limit R P0,2 .
  • NSR Sharpp-Notch Strength-to-Yield Strength Ratio
  • the static mechanical characteristics in other words the ultimate ultimate tensile strength R m , the tensile yield strength R p0,2 and the elongation at break A, are determined by a tensile test. according to standard EN 10002-1 or NF EN ISO 6892-1, the location to which the parts are taken and their meaning being defined by the EN 485-1 standard.
  • the notched specimen mechanical strength is obtained in accordance with ASTM E602-03.
  • the so-called NSR ratio between notched specimen strength and yield strength R P0.2 (“Sharp-Notch Strength-to-Yield Strength Ratio" is calculated. report gives an indication of the notch resistance of the sample.
  • the problem is solved by an alloy comprising (in% by weight); Zn : 5.4 - 5.8 % , mg : 0.8 - 1.8 % Cu : ⁇ 0.2 % , Zr : 0.05 - 0.08 % , Ti ⁇ 0.15 % , mn ⁇ 0.1 % , Cr ⁇ 0.1 % , Yes ⁇ 0.15 % , Fe ⁇ 0.20 % , impurities with an individual content ⁇ 0.05% each and ⁇ 0.15% in total, remains aluminum.
  • the combination of the zinc content of 5.4 - 5.8% by weight, the magnesium content of 0.8 to 1.8% and the copper content of less than 0.2% by weight makes it possible to achieve an improved compromise between mechanical strength and notch resistance.
  • the preferred magnesium content is 1.0 to 1.4% by weight or even 1.1 to 1.3% by weight.
  • the preferred copper content is less than 0.05% by weight or even less than 0.04% by weight.
  • the zirconium content is 0.05 to 0.08% by weight, so as to further reduce the quenching sensitivity of the thick aluminum blocks.
  • the titanium content is less than 0.15% by weight.
  • an amount of titanium of between 0.01 and 0.05% by weight and preferably between 0.02 and 0.04% by weight is added in order to refine the grain size during casting.
  • the Cr content and the Mn content are less than 0.1%.
  • the Cr content is less than 0.05% by weight or even less than 0.03% by weight, and / or the Mn content is less than 0.05% by weight or even less than 0, 03% by weight, which allows in particular to further reduce the sensitivity to quenching thick aluminum blocks.
  • Si and Fe are unavoidable impurities whose content is to be minimized so as in particular to improve the mechanical strength on the notched specimen.
  • the Fe content is less than 0.20% by weight and preferably less than 0.15% by weight.
  • the Si content is less than 0.15% by weight and preferably less than 0.10% by weight.
  • the casting of the thick block is preferably carried out by semi-continuous casting with direct cooling ("Direct Chill Casting").
  • the thick block has a thickness greater than 350 mm, and preferably greater than 450 mm or even greater than 550 mm.
  • the block is essentially parallelepipedal in shape, it generally has a larger dimension (length), a second larger dimension (width) and a smaller dimension (thickness).
  • the block may optionally then be homogenized, typically by a heat treatment at a temperature between 450 and 550 ° C for a period of 10 minutes to 30 hours and / or undergo a flash treatment at a temperature between 300 and 400 ° C for a period of 10 minutes to 30 hours followed by cooling to a temperature below 100 ° C.
  • the block is then put into solution, that is to say heat-treated so that the block temperature reaches 500 to 560 ° C for a period of between 10 minutes and 5 hours, or even 20 hours.
  • This heat treatment can be carried out at a constant temperature or in several stages.
  • the block After dissolution, the block is cooled to a temperature below 100 ° C, preferably to room temperature.
  • the cooling rate is at least 800 ° C / h.
  • Such a cooling rate can be obtained by spraying or immersion in water. Since a cooling rate that is too high can generate excessive residual stresses in the blocks, water is preferably used at a temperature of at least 50.degree. C. and preferably at least 70.degree. C. for cooling.
  • the block thus hardened is stripped, preferably by cold compression with a permanent deformation rate of between 1% and 5% and preferably between 2 and 4%. The stress relieving allows to reduce the residual stresses in the metal and to avoid the deformations during the machining.
  • the income is made so that the block reaches a temperature of 120 and 170 ° C and preferably between 130 and 160 ° C for a period of 4 to 48 hours and preferably between 8 and 24 hours.
  • an income is achieved to reach the T6 or T652 state, corresponding to the peak of the static mechanical properties (Rm and Rp0,2).
  • said block does not undergo between the casting and the significant deformation step income by wrought.
  • wrought is typically meant rolling operations or hot forging.
  • significant deformation is meant that none of the dimensions of the cast block - which is a thick block of substantially parallelepiped shape (length L, width TL, thickness TC) - undergoes significant modification, that is to say typically at least about 10%, by heat treatment between casting and income.
  • the thick blocks obtained by the process according to the invention have a compromise of advantageous properties, in particular between the elastic limit and the notch resistance, which are two antagonistic properties (the more important one is, the more other is weak). More specifically, the Applicant has found that for a thick block of an alloy having the composition according to the invention and having been obtained by following the claimed process steps until the income (casting, homogenization and stress relief optional, dissolution and quenching without significant wrought between the casting and the final step of income), regardless of the income treatment (mono- or multi-level) subsequently carried out to reach a given elastic limit Rp0.2, the NSR (“Sharp-Notch Strength-to-Yield Strength Ratio") parameter used to characterize the notch resistance of the block thus obtained, reaches a value that does not depend on the income treatment performed to obtain the targeted Rp02. For such thick blocks, a relationship between the RpO 2 and the NSR measured for example at 1 ⁇ 4 of the thickness can therefore be established, and this relationship appears to be substantially linear.
  • the NSR
  • the Applicant has been able to establish that the notch resistance, as evaluated at 1 ⁇ 4 thickness in the TL direction by the NSR (measured according to ASTM E602-03, paragraph 9.2) is greater than: - 0,017 * R p 0.2 + 6.7.
  • the NSR is at least 0.8, preferably 1.0, and the yield strength is at least 320 MPa and preferably 330 MPa.
  • Table 1 Chemical composition (% by weight) ⁇ / u> Reference Yes Fe Cu mn mg Zn Zr Cr Ti AT 0.05 0.08 0.02 0.01 1.2 5.7 0.08 ⁇ 0.01 0.04 B 0.05 0.08 0.03 ⁇ 0.01 1.2 5.6 0.08 ⁇ 0.01 0.04 VS 0.05 0.13 0.2 0.01 2.8 4.9 0.09 ⁇ 0.01 0.03 D 0.08 0.04 0.6 ⁇ 0.01 2.2 6.3 0.10 ⁇ 0.01 0.03
  • Alloys A, B, C and D were cast as blocks of thickness 625 mm.
  • the blocks of alloys A and C were transformed as follows: the blocks were first homogenized at 10h 480 ° C. The blocks were then dissolved for 4 hours at 540 ° C. and air-cooled at approximately 40 ° C./h (from 540 ° C. to 410 ° C. in 2 hours and then from 410 ° C. to 90 ° C. in 9 hours). ). The blocks were then first treated at 105 ° C for about 12 hours and then at 160 ° C for about 16 hours.
  • the alloy blocks B and D were transformed as follows: the blocks first underwent a 2 hour expansion at 350 ° C. After being dissolved for 4 hours at 540 ° C. (Block B) or 10 hours at 475 ° C. (Block D), the blocks were cooled with water at 80 ° C. by immersion. The blocks then underwent compression straightening of 3%. The alloy blocks B were then tempered at 130 ° C for 24 h (block B1) or 150 ° C for 16 h (block B2). The alloy block D was first treated at 90 ° C for 8 to 12 hours and then at 160 ° C for 14 to 16 hours.
  • the Figure 1 presents the compromise obtained between the elastic limit R P0,2 and the report called “Sharp-Notch Strength-to-Yield Strength Ratio", known under the abbreviation "NSR" and commonly used to characterize the sensitivity to the effect notch of a material.
  • NSR Storage-Notch Strength-to-Yield Strength Ratio
  • this parameter is the ratio between the mechanical strength measured on notched specimen and the elastic limit measured on non-notched specimen.
  • ASTM E602-03 particularly in section 9.2.
  • the alloy A allows, with respect to the alloy C, a simultaneous improvement in the yield strength and in the NSR ratio, and thus in the notch strength.
  • the NSR report obtained is greater than -0.017 R p0.2 + 6.4.
  • the process for converting the alloy according to the invention makes it possible to further improve the NSR ratio.
  • the alloy block B according to the invention has an NSR ratio greater than -0.017 * R p0.2 + 6.7.

Claims (6)

  1. Verfahren zur Herstellung eines Aluminiumblocks mit einer Dicke von mehr als 350 mm, umfassend die Schritte:
    (a) Gießen eines dicken Blocks aus einer Aluminiumlegierung mit (in Gew.-%): Zn: 5,4 - 5,8 %, Mg: 0,8 - 1,8 %, Cu: < 0,2 %, Zr: 0,05- 0,08 %, Ti: < 0,15 %, Mn: < 0,1 %, Cr: < 0,1 %, Si: < 0,15 %, Fe: < 0,20 %,
    Verunreinigungen mit einem jeweiligen Gehalt < 0,05 % und < 0,15 % insgesamt, Rest Aluminium;
    b) gegebenenfalls Homogenisieren bei einer Temperatur zwischen 450 und 550°C für 10 Minuten bis 30 Stunden und/oder Entspannen bei einer Temperatur zwischen 300 und 400°C für 10 Minuten bis 30 Stunden mit anschließendem Abkühlen auf eine Temperatur unter 100°C;
    (c) Lösungsglühen des gegossenen Blocks bei einer Temperatur von 500 bis 560°C für 10 Minuten bis 20 Stunden,
    (d) Abkühlen des lösungsgeglühten Blocks auf eine Temperatur unter 100°C mit einer Abkühlgeschwindigkeit von mindestens 800°C/h und Spannungsarmmachen des lösungsgeglühten und abgekühlten Blocks durch kontrolliertes Stauchen mit einer bleibenden Verformung zwischen 1 und 5 %,
    (e) Auslagern des lösungsgeglühten und gekühlten Blocks durch Erwärmen auf 120 bis 170°C für 4 bis 48 Stunden,
    bei dem keine der Dimensionen des gegossenen Blocks eine Verformung von mindestens 10 % durch Umformung zwischen den Schritten Gießen und Auslagern erfährt.
  2. Verfahren nach Anspruch 1, bei dem der lösungsgeglühte und abgekühlte Block durch kontrolliertes Stauchen mit einer bleibenden Verformung zwischen 2 und 4 % spannungsarm gemacht wird.
  3. Verfahren nach Anspruch 2, bei dem das Abkühlen aus Schritt (d) durch Besprühen mit oder Eintauchen in Wasser bei einer Temperatur von mindestens 50°C und vorzugsweise mindestens 70°C durchgeführt wird.
  4. Aluminiumblock mit einer Dicke von mehr als 350 mm, der durch das Verfahren nach irgendeinem der Ansprüche 1 bis 3 gewonnen werden kann,
    wobei der Block aufweist (in Gew.-%): Zn: 5,4 - 5,8 %, Mg: 0,8 -1,8, Cu: < 0,2 %, Zr: 0,05 - 0,08 %, Ti: < 0,15 %, Mn: < 0,1 %, Cr: < 0,1 %, Si: < 0,15 %, Fe: < 0,20 %, Verunreinigungen mit einem jeweiligen Gehalt < 0,05 % und < 0,15 % insgesamt, Rest Aluminium,
    und dadurch gekennzeichnet ist, dass bei ¼ Dicke in TL-Richtung die Dehngrenze Rp0,2, ausgedrückt in MPa, und das nach ASTM E602-03, Absatz 9.2 gemessene Verhältnis NSR zwischen der Kerbschlagprobenfestigkeit und der Dehngrenze Rp0,2 so sind, dass:
    - NSR > -0,017 * Rp0,2 + 6,7 und
    - Rpo,2 > 320 MPa, vorzugsweise 330 MPa.
  5. Aluminiumblock nach Anspruch 4, dadurch gekennzeichnet, dass NSR > 0,8, vorzugsweise 1,0.
  6. Verwendung eines dicken Blocks nach einem der Ansprüche 4 bis 5 zur Herstellung von Spritzgießformen für Kunststoffe.
EP11808242.9A 2010-12-14 2011-12-06 Dicke produkte aus 7xxx-legierungen und deren herstellungsverfahren Active EP2652163B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL11808242T PL2652163T3 (pl) 2010-12-14 2011-12-06 Grube produkty ze stopu 7xxx i sposób wytwarzania

Applications Claiming Priority (2)

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FR1004865A FR2968675B1 (fr) 2010-12-14 2010-12-14 Produits epais en alliage 7xxx et procede de fabrication
PCT/FR2011/000637 WO2012080592A1 (fr) 2010-12-14 2011-12-06 Produits epais en alliage 7xxx et procede de fabrication

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EP2652163A1 EP2652163A1 (de) 2013-10-23
EP2652163B1 true EP2652163B1 (de) 2018-09-19

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US (2) US11306379B2 (de)
EP (1) EP2652163B1 (de)
JP (1) JP6118728B2 (de)
KR (1) KR101900973B1 (de)
CA (1) CA2820768A1 (de)
CL (1) CL2013001716A1 (de)
FR (1) FR2968675B1 (de)
MX (1) MX354911B (de)
PL (1) PL2652163T3 (de)
WO (1) WO2012080592A1 (de)

Cited By (2)

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US10835942B2 (en) 2016-08-26 2020-11-17 Shape Corp. Warm forming process and apparatus for transverse bending of an extruded aluminum beam to warm form a vehicle structural component
US11072844B2 (en) 2016-10-24 2021-07-27 Shape Corp. Multi-stage aluminum alloy forming and thermal processing method for the production of vehicle components

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CN105339515A (zh) * 2013-09-30 2016-02-17 苹果公司 具有高强度和外表吸引力的铝合金
US20150368772A1 (en) * 2014-06-19 2015-12-24 Apple Inc. Aluminum Alloys with Anodization Mirror Quality
US10208371B2 (en) 2016-07-13 2019-02-19 Apple Inc. Aluminum alloys with high strength and cosmetic appeal
US11345980B2 (en) 2018-08-09 2022-05-31 Apple Inc. Recycled aluminum alloys from manufacturing scrap with cosmetic appeal
WO2020263864A1 (en) * 2019-06-24 2020-12-30 Arconic Technologies Llc Improved thick wrought 7xxx aluminum alloys, and methods for making the same
FR3118632B1 (fr) * 2021-01-05 2023-09-29 Airbus Operations Sas Procédé d’optimisation des propriétés en corrosion d’un assemblage d’au moins deux pièces réalisées en alliage à base d’aluminium assemblées par soudage par friction.
CN112981289B (zh) * 2021-04-21 2021-08-03 中国航发北京航空材料研究院 一种7000系铝合金铸锭去应力退火及均匀化退火的方法
CN113528866B (zh) * 2021-06-16 2022-05-20 天津忠旺铝业有限公司 一种航空用高强耐腐蚀7xxx铝合金板材的制备方法
CN115011850A (zh) * 2022-05-10 2022-09-06 慈溪市宜美佳铝业有限公司 一种不易变形的铝型材及其淬火工艺

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US10835942B2 (en) 2016-08-26 2020-11-17 Shape Corp. Warm forming process and apparatus for transverse bending of an extruded aluminum beam to warm form a vehicle structural component
US11072844B2 (en) 2016-10-24 2021-07-27 Shape Corp. Multi-stage aluminum alloy forming and thermal processing method for the production of vehicle components

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KR20140012628A (ko) 2014-02-03
JP6118728B2 (ja) 2017-04-19
US20130284322A1 (en) 2013-10-31
EP2652163A1 (de) 2013-10-23
FR2968675A1 (fr) 2012-06-15
WO2012080592A1 (fr) 2012-06-21
MX354911B (es) 2018-03-26
CA2820768A1 (fr) 2012-06-21
KR101900973B1 (ko) 2018-09-20
US11306379B2 (en) 2022-04-19
MX2013006848A (es) 2013-11-01
FR2968675B1 (fr) 2013-03-29
PL2652163T3 (pl) 2019-05-31
JP2014505786A (ja) 2014-03-06
US20220389558A1 (en) 2022-12-08
CL2013001716A1 (es) 2013-12-06

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