EP3294918B1 - Procédé de vieillissement thermique à quatre étapes pour l'amélioration de la résistance à la fissuration influencée par l'environnement d'alliages d'aluminium de série 7xxx - Google Patents

Procédé de vieillissement thermique à quatre étapes pour l'amélioration de la résistance à la fissuration influencée par l'environnement d'alliages d'aluminium de série 7xxx Download PDF

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EP3294918B1
EP3294918B1 EP16831924.2A EP16831924A EP3294918B1 EP 3294918 B1 EP3294918 B1 EP 3294918B1 EP 16831924 A EP16831924 A EP 16831924A EP 3294918 B1 EP3294918 B1 EP 3294918B1
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samples
alloys
nacl
temperature
aged
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EP3294918A1 (fr
EP3294918B8 (fr
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Indian Institute of Technology Bombay
Godrej and Boyce Manufacturing Co Ltd
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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
    • 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor

Definitions

  • This invention relates to a four-step thermal aging method for improving environmentally assisted cracking resistance of 7xxx series aluminium alloys.
  • Aluminium alloys find extensive use across a wide range of applications from structures to household appliances. Low cost, light weight, versatility and recyclability are some of the main advantages of aluminium alloys. Various grades of aluminium alloys are available depending mainly on their end use and requirement. AA 7xxx or AA 7000 series aluminium alloys such as AA 7010, AA 7050, and AA 7085 are characterized by their high strength and high environmentally assisted cracking resistance and are extensively used for structural applications in aerospace and armor industries.
  • SCC Stress corrosion cracking
  • HE hydrogen embrittlement
  • EAC environmentally assisted cracking
  • the 7xxx series alloys are subjected to various thermal aging treatments in order to enhance their strength and EAC resistance.
  • T C Tsai T H Chuang, Atmospheric stress corrosion cracking of a superplastic 7475 aluminum alloy, Metall Mater Trans A 27 (1996) 2617-2627 ;
  • Solutionizing of the alloys is a pretreatment for thermal aging.
  • the precipitates that evolve will impede the dislocation movement in the material and impart strength to the alloys.
  • the precipitates that evolve in the grain boundary of the alloys impart EAC resistance to the alloys.
  • the grain boundary precipitates are mainly Mg (Zn,Al,Cu) 2 complexes which are highly anodic in nature. Since Mg is a very active anodic element, the grain boundary precipitates can undergo selective dissolution in the corrosive environments adversely affecting the grain boundary cohesive strength of the alloys. In the presence of stresses, such dissolution can lead to intergranular brittle fracture of the alloys.
  • the rate of intergranular stress corrosion cracking is higher if such anodic precipitates are located continuously at grain boundary.
  • the various thermal aging treatments known and reported in the prior art as stated above do not impart sufficient strength and EAC resistance to the alloys for high strength applications, especially in the aerospace and armor industries and it is still desirable to have aluminium alloys having improved strength and EAC resistance for such applications.
  • a four-step thermal aging method for improving environmentally assisted cracking resistance of 7xxx series aluminium alloys comprising solutionizing and aging 7xxx series aluminium alloys, wherein the aging is carried out by treating the alloys at a temperature of 120 to 130°C for 0.3 to 0.5h, water quenching the alloys to a temperature of 25 to 27°C and further treating the alloys at a temperature of 80 to 95°C for 100 to 120h and at a temperature of 120 to 130°C for 20 to 24h and at a temperature of 155 to 160°C for 1 to 5h and air cooling the alloys to room temperature, sequentially.
  • the four-stage thermal aging of the aluminium alloys employing temperature cycles sequentially as described above according to the invention assist in bringing about novel microstructural changes in the alloys so as to improve the EAC resistance of the alloys. It is quite evident from the experimental studies that follow that according to the method of invention more copper is diffused into the grain boundary of the alloys and the distance between the grain boundary precipitates is increased.
  • the copper enrichment and the discontinuously located grain boundary precipitates produce microstructures that significantly reduce the anodic dissolution of the grain boundary precipitates and increase the EAC resistance of the alloys in corrosive environments (especially in 3.5wt.% NaCl).
  • the aging cycles also aid to nucleate more precipitates at the grain matrix and increase the strength levels of the alloys.
  • the thermally aged aluminium alloys of the invention are ideal for high strength applications, especially in the aerospace and armor industries because of their excellent EAC resistance and higher strength. However, they can be used in any other applications also.
  • the following experimental examples are illustrative of the invention but not limitative of the scope thereof:
  • the experiments were conducted on dog-bone shaped tensile specimens of AA 7010, AA 7050 and AA 7085 prepared according to ASTM E8. Prior to thermal aging, the alloy samples were solutionzied at 460°C and water quenched in known manner. The thermal aging of the samples was carried out in a laboratory scale oil bath furnace fitted with temperature control of accuracy ⁇ 2°C. Slow strain rate tests (SSRT) were carried out at a strain rate of 10 -6 s -1 and 10 -7 s -1 . Gauge length of the specimens was continuously exposed to 3.5 wt% NaCl that was freely exposed to air, till failure. Each experiment was at least triplicated.
  • the electrical conductivity of the heat treated samples were measured using an EDDY current type conductivity meter. EAC susceptibility of the samples was evaluated based on elongation and ultimate tensile strength (UTS) of the samples measured in air (considered as inert) and in corrosive environment (3.5 wt% NaCl freely exposed to air).
  • Fractured samples from SSRT were ultrasonicated in acetone immediately after the failure and were dried and examined under a scanning electron microscope (SEM) to determine the mode of fracture. Ductility (% elongation) of the samples was calculated by measuring the gauge length of the failed samples manually. Microstructures of the specimens were examined in a field emission transmission electron microscope (FEG TEM) operating at 200 kV.
  • FEG TEM field emission transmission electron microscope
  • AA 7010 samples in as-received condition were used in the study.
  • a few of the as-received samples were subjected to T6 (peak aged) and T7451 (over aged) temper treatments by us according to the temperature cycles as given in the following Table 2:
  • Table 2 Thermal treatment Temperature cycle Peak aged (PA) Aged at 100°C for 8 h and further aged at 120°C for 8 h and air cooled
  • Over aged (OA) Aged at 100°C for 8 h and further aged at 120°C for 8 h and at 170°C for 8 h and air cooled
  • Table 4 shows that the peak aged samples showed an elongation of about 7.5% in 3.5 wt% NaCl against about 13.7% in air.
  • the drop of elongation in NaCl was about 6.2%.
  • the over aged samples showed an elongation of about 12% in 3.5 wt% NaCl against about 13.6% in air.
  • the drop of elongation in NaCl was about 1.6% compared to air.
  • the samples treated according to the invention showed an elongation of about 14% in 3.5 wt% NaCl against about 15% in air.
  • the drop of elongation in NaCl was only about 1% compared to air.
  • the peak aged samples reached a UTS (ultimate tensile strength) value of about 577 MPa in air compared to about 548 MPa in 3.5wt% NaCl.
  • the drop in strength in 3.5wt% NaCl was about 69 MPa.
  • the over aged samples reached a UTS value of about 539 MPa in air compared to about 530 MPa in 3.5wt% NaCl.
  • the drop in strength in 3.5wt% NaCl was about 9 MPa.
  • the samples according to the invention showed an increased UTS value upto about 580MPa in air and upto about 569 MPs in NaCl.
  • the drop of UTS value in NaCl was about 11 MPa
  • the increase in the elongation and UTS values of the samples treated according to the invention are significant and substantial in the overall structural strength and EAC resistance of the 7xxx series aluminium alloys in 3.5 wt% NaCl.
  • the increase or improvement in the elongation and UTS values are indicative of the changes in the microstructures of the samples treated according to the invention.
  • the graph in Fig 1 of the drawings is a representation of stress against % elongation of the alloys in 3.5 wt% NaCl.
  • the graph in Fig 1 supports the findings in Table 4.
  • Table 5 shows that the alloy samples treated according to the invention had a lower electrical conductivity as compared to OA samples but had improved EAC resistance as shown by Table 4 above.
  • Fractographs or fracture surface maps taken at the edges of the samples treated as per PA and OA temper conditions and according to the invention and failed in 3.5 wt% NaCl were as shown in Figs 2a , 2b and 2c of the drawings, respectively.
  • the peak aged samples of AA7010 in Fig 2a shows extensive intergranular cleavage fracture having brittle facets indicative of stress corrosion cracking (SCC) failure.
  • SCC stress corrosion cracking
  • Table 4 supports this finding in terms of drop in ductility (% elongation) .
  • the over aged samples in Fig 2b and the samples according to the invention in Fig 2c did not show any signs of intergranular SCC failure.
  • the samples treated according to the invention showed enhanced elongation and strength values even under 3.5 wt.% NaCl clearly indicating that the samples treated according to the invention had better EAC resistance.
  • TEM micrographs of the AA 7010 samples peak aged, over aged and treated according to the invention were taken in a FEG TEM and were as shown in Figs 3a, 3b and 3c of the drawings, respectively.
  • the peak aged samples of Fig 3a show finer matrix precipitates and continuous network of fine grain boundary precipitates
  • the over aged samples of Fig 3b show coarse matrix precipitates and relatively coarser and discontinuous network of grain boundary precipitates.
  • the samples of Fig 3c treated according to the invention show that the grain matrix precipitates remained finer whilst the grain boundary precipitates became coarser thereby improving the strength of the samples.
  • AA 7050 samples in as-received condition were used for the study.
  • the samples as-received were already treated according to T7451 (OA temper condition).
  • a few of the samples were further subjected to thermal aging according to the invention under the same conditions as given in Table 3 of Example 1.
  • the as-received and over aged samples showed an elongation of about 13.92 % in 3.5 wt% NaCl against about 15.25 % elongation in air.
  • the as-received and over aged samples had a UTS value of about 523 MPa in air compared to about 511 MPa in 3.5 wt% NaCl.
  • the samples treated as per the invention showed about 16.36% elongation in air and about 15.18% elongation in 3.5 wt% NaCl.
  • the samples treated as per the invention showed a UTS value of about 600 MPa in air and about 597 MPa in NaCl.
  • the samples treated according to the invention exhibited significant improvement in the strength and EAC resistance as compared to the over aged samples even at a strain rate of 10 -7 /s.
  • Table 7 shows that the alloy samples treated according to the invention had a lower electrical conductivity as compared to OA samples but had improved EAC resistance as shown by Table 6 above.
  • TEM micrographs of the as-received and over aged samples and samples treated according to the invention were taken in a FEG TEM and were as shown in Figs 7a and 7b of the drawings respectively.
  • the as-received and over aged samples of Fig 7a show a discontinuous network of grain boundary precipitates, whereas the treated samples of Fig 7b show a relatively coarser and more discontinuous grain boundary precipitates.
  • a graphical representation of % Cu in the grain boundary precipitates of the samples taken through FEG TEM is shown in Fig 8 of the drawings.
  • the grain boundary precipitates of the over aged alloys and alloys treated as per the invention showed 3.4 and 5.3 wt% Cu respectively.
  • the microstructural changes in the grain boundary precipitates are understood to be the reasons or causative factors for the improved EAC resistance of the treated samples.
  • AA 7085 samples in as-received condition were used for the study.
  • the samples as-received were already thermally treated according to T7651 (OA temper condition).
  • a few of the samples were further treated according to the invention under the same conditions as given in Table 3 of Example 1.
  • the SSRT results for the AA 7085 samples in as-received and over aged condition and after the thermal treatment according to the invention in 3.5 wt% NaCl were as shown in Table 8 below.
  • Table 8 Samples 3.5 wt% NaCl UTS (in MPa) % Elongation As-received and over aged 10 -6 s -1 500 5.5 ⁇ 0.2 10 -7 s -1 485 3.3 ⁇ 0.4 Treated as per invention 10 -6 s -1 520 8 ⁇ 0.8 10 -7 s -1 498 7 ⁇ 0.6
  • the as-received and over aged samples showed an elongation of about 5.5 % at a strain rate of 10 -6 s -1 , whereas the elongation dropped to about 3.3 % at a strain rate of 10 -7 s -1 in 3.5 wt% NaCl.
  • the samples treated as per the invention showed high strain to failure at the strain rate of 10 -6 s -1 and even at the strain rate of 10 -7 s -1 in 3.5 wt.% NaCl indicating that the samples treated as per the invention had significantly increased the EAC resistance.
  • the samples treated as per the invention also had significantly higher strength (MPa) values.
  • the graphical representation of stress vs % elongation of the samples in 3.5 wt.% NaCl as shown in Fig 9 of the drawings supports the finding in Table 8.
  • TEM micrographs of the as-received and over aged samples and samples treated according to the invention were taken in a FEGTEM and the images were as shown in Figs 11a and 11b of the drawings respectively.
  • the as-received and over aged samples in Fig 11a show a discontinuous network of grain boundary precipitates, whereas the samples treated as per the invention in Fig 11b show a relatively coarser and more discontinuous grain boundary precipitates.
  • the microstructural changes in the grain boundary precipitates are understood to be the reasons or causative factors for the improved EAC resistance of the treated samples as per invention.
  • the method of the invention is unique, innovative and inventive.
  • the method of the invention has been found to be effective in 7xxx aluminium alloys having a wide range of quench sensitivity. Therefore, it is believed that the method of the invention is applicable to at least all the 7000 series aluminium alloys, if not aluminium alloys in general.

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  • Crystallography & Structural Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
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Claims (3)

  1. Procédé de vieillissement thermique en quatre étapes pour l'amélioration de la résistance à la fissuration favorisée par l'environnement d'alliages d'aluminium de la série 7xxx, comprenant une traitement thermique en solution et le vieillissement d'alliages d'aluminium de la série 7xxx, dans lequel le vieillissement est effectué par traitement des alliages à une température de 120 à 130 °C pendant 0,3 à 0,5 h, trempe à l'eau des alliages jusqu'à une température de 25 à 27 °C et traitement encore des alliages à une température de 80 à 95 °C pendant 100 à 120 h et à une température de 120 à 130 °C pendant 20 à 24 h et à une température de 155 à 160 °C pendant 1 à 5 h et refroidissement à l'air des alliages jusqu'à la température ambiante, successivement.
  2. Procédé tel que revendiqué dans la revendication 1, dans lequel les alliages sont traités à une température de 130 °C pendant 0,5 h, trempés à l'eau jusqu'à 27 °C et encore traités à une température de 85 °C pendant 120 h, à une température de 130 °C pendant 24 h et à une température de 157 °C pendant 2,5 h.
  3. Procédé tel que revendiqué dans la revendication 1 ou 2, dans lequel les alliages sont AA 7010, AA 7050 et AA 7085.
EP16831924.2A 2016-08-04 2016-11-30 Procédé de vieillissement thermique à quatre étapes pour l'amélioration de la résistance à la fissuration influencée par l'environnement d'alliages d'aluminium de série 7xxx Not-in-force EP3294918B8 (fr)

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IN201621026704 2016-08-04
PCT/IN2016/000280 WO2018025275A1 (fr) 2016-08-04 2016-11-30 Procédé de vieillissement thermique à quatre étapes pour l'amélioration de la résistance à la fissuration influencée par l'environnement d'alliages d'aluminium de série 7xxx

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CN112218963B (zh) * 2018-07-02 2022-09-20 奥托福克斯两合公司 铝合金以及由这种合金制造的过老化的铝合金产品

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US4477292A (en) 1973-10-26 1984-10-16 Aluminum Company Of America Three-step aging to obtain high strength and corrosion resistance in Al-Zn-Mg-Cu alloys
US4431467A (en) 1982-08-13 1984-02-14 Aluminum Company Of America Aging process for 7000 series aluminum base alloys
JP3705320B2 (ja) * 1997-04-18 2005-10-12 株式会社神戸製鋼所 耐食性に優れる高強度熱処理型７０００系アルミニウム合金
AUPQ485399A0 (en) 1999-12-23 2000-02-03 Commonwealth Scientific And Industrial Research Organisation Heat treatment of age-hardenable aluminium alloys
IL156386A0 (en) * 2000-12-21 2004-01-04 Alcoa Inc Aluminum alloy products and artificial aging method
JP2003213387A (ja) * 2002-01-22 2003-07-30 Mitsubishi Heavy Ind Ltd 航空機用ロール成形部品の製造方法
JP5343333B2 (ja) * 2007-07-06 2013-11-13 日本軽金属株式会社 耐応力腐食割れ性に優れた高強度アルミニウム合金材の製造方法
US8333853B2 (en) 2009-01-16 2012-12-18 Alcoa Inc. Aging of aluminum alloys for improved combination of fatigue performance and strength
US9249487B2 (en) 2013-03-14 2016-02-02 Alcoa Inc. Methods for artificially aging aluminum-zinc-magnesium alloys, and products based on the same
US9765419B2 (en) 2014-03-12 2017-09-19 Alcoa Usa Corp. Methods for artificially aging aluminum-zinc-magnesium alloys, and products based on the same
CN104962847B (zh) * 2015-07-16 2016-11-16 中南大学 一种提高7系合金厚板均匀性和抗腐蚀性能的热处理工艺

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US20190153578A1 (en) 2019-05-23
WO2018025275A1 (fr) 2018-02-08
EP3294918B8 (fr) 2019-02-27

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