CN104451291A - Homogenizing heat treatment process of Er and Zr composite microalloyed Al-Zn-Mg-Cu alloy - Google Patents

Homogenizing heat treatment process of Er and Zr composite microalloyed Al-Zn-Mg-Cu alloy Download PDF

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CN104451291A
CN104451291A CN201410676636.8A CN201410676636A CN104451291A CN 104451291 A CN104451291 A CN 104451291A CN 201410676636 A CN201410676636 A CN 201410676636A CN 104451291 A CN104451291 A CN 104451291A
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alloy
heat treatment
treatment process
homogenizing heat
homogenizing
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CN104451291B (en
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聂祚仁
吴浩
文胜平
高坤元
黄晖
吴晓蓝
王为
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Beijing University of Technology
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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

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Abstract

The invention discloses a homogenizing heat treatment process of an Er and Zr composite microalloyed Al-Zn-Mg-Cu alloy, and belongs to the technical field of metal alloy materials. The invention particularly relates to a homogenizing heat treatment process of aluminum alloy cast ingot with alloy components comprising 7.2-8.2% of Zn, 2.0-3.0% of Mg, 0.4-0.8% of Cu, 0.2-0.5% of Mn, 0.1-0.15% of Er, 0.1-0.15% of Zr, not greater than 0.3% of inevitable impurities and the balance of Al. The homogenizing heat treatment process comprises the following process: a single-stage homogenizing heat treatment process of preserving the heat for 2-48 hours at 450-490 DEG C; a double-stage homogenizing heat treatment process of preserving the heat for 6-10 hours at 400 DEG C and then preserving the heat for 24-48 hours at 470 DEG C. The homogenizing heat treatment process can be used for eliminating the defects of an alloy as-cast structure, improving the homogeneity and the hot-working performances of the alloy tissue, promoting the separation and the growth of A13 (Er, Zr) heat-resistant dispersed phase in the alloy, and is beneficial to improvement of the recrystallization resistance and restraining deformed crystalline grains from being grown in a hot processing process of the alloy.

Description

A kind of homogenizing heat treatment of Er, Zr combined microalloying Al-Zn-Mg-Cu alloy
Technical field
The invention belongs to metal alloy compositions technical field, be specifically related to a kind of single-stage and two-step homogenization thermal treatment process of Al-Zn-Mg-Cu-Er-Zr alloy.
Technical background
It is low that Al-Zn-Mg-Cu aluminum alloy has density, and intensity is high, toughness, and hot workability and the feature such as corrosion resistance nature is better, be widely used in the fields such as aerospace, shipping industry, communications and transportation, becoming one of primary structural material.But due to Al-Zn-Mg-Cu alloy degree higher, the uneven of serious dendritic segregation, intracrystalline and Grain Boundary Chemistry Composition and structure distribution is there is in process of setting, these all seriously can fall low-alloyed plasticity, worsen hot workability, alloy product intensity and plasticity are reduced, and anisotropy and corrosion susceptibility increase.Therefore in order to eliminate the impact of ingot structure defect alloy properties for follow, before ingot casting thermal distortion, rational homogenizing thermal treatment must be carried out.
Homogenizing thermal treatment is an extremely important technological process of reasonable offer and application.Rational homogenizing thermal treatment can reach following effect: 1), eliminate each element segregation in alloy cast ingot, each element is uniformly distributed; 2), eliminate low melting point eutectic phase in alloy, put forward heavy alloyed hot workability; 3) the infusibility phase, in nodularization alloy and not melt-phase, improve alloy properties for follow; 4), separate out small and dispersed particle, suppress deforming alloy recrystallize and grain growth.Therefore for this type of containing the Al-Zn-Mg-Cu alloy of micro alloying element Er, Zr, its homogenizing heat treatment be applicable to not only needs to eliminate component segregation and the once phase of alloy cast ingot, also needs by homogenizing thermal treatment simultaneously, separates out the Al of small and dispersed 3(Er, Zr) particle improves the follow-up performance of alloy.The present invention is that devising this alloy phase should suitable single-stage and two-step homogenization thermal treatment process on above technical background basis.
Summary of the invention
The object of the present invention is to provide the single-stage homogenizing and two-step homogenization thermal treatment process that are applicable to Al-Zn-Mg-Cu-Er-Zr alloy (the 7xxx line aluminium alloy containing Er, Zr).Provide treatment process not only can eliminate the casting flaw of ingot casting, improve Al-Zn-Mg-Cu-Er-Zr alloy hot workability, and thermally-stabilised phase Al can be promoted 3the precipitation of (Er, Zr) particle, contributes to improving alloy and grows up in the anti-recrystallizing performance of hot procedure and suppression deformed grains.
The invention provides and be applicable to Al-Zn-Mg-Cu-Er-Zr alloy single-stage and two-step homogenization thermal treatment process, it is (weight percent) Zn7.2 ~ 8.2, Mg2.0 ~ 3.0, Cu0.4 ~ 0.8, Mn0.2 ~ 0.5, Er0.1 ~ 0.15, Zr0.1 ~ 0.15, inevitable impurity≤0.3 that its technique is applicable to each component of alloy, surplus is the aluminium alloy cast ingot of Al, its composition is preferably: 7.27%Zn, 2.32%Mg, 0.6%Cu, 0.29%Mn, 0.11%Er, 0.13%Zr, impurity <0.2%, surplus is Al.
Provided by the present invention for being applicable to Al-Zn-Mg-Cu-Er-Zr alloy single-stage and two-step homogenization thermal treatment process, its technique comprises the following steps:
1), the thermal treatment of single-stage homogenizing is: be incubated 2 ~ 48h after alloy cast ingot is warming up to 450 ~ 490 DEG C respectively; Its optimize single-stage homogenizing heat treating regime be after being incubated 24 ~ 48h at 470 DEG C air cooling to room temperature, as shown in Figure 1a.
2), two-step homogenization thermal treatment is: alloy cast ingot is warming up to 400 DEG C of insulation 6 ~ 10h, and after continuing to be warming up to 470 DEG C of insulation 24 ~ 48h subsequently, air cooling is to room temperature, as shown in Figure 1 b.
Single-stage Homogenization Treatments technique of the present invention can greatly eliminate alloy of ingot segregation, alloying constituent is evenly distributed, eliminate the low melting point phase in alloy and the infusibility phase in nodularization alloy, can put forward heavy alloyed follow-up hot workability, this single-stage Homogenization Treatments technique can separate out the Al of small and dispersed simultaneously 3(Er, Zr) particle.
Two-step homogenization treatment process of the present invention is further perfect on this single stage process basis, and its first step, at 400 DEG C of heating and thermal insulations, is conducive to the precipitation of the microalloy element such as Er, Zr in alloy, facilitates thermally-stabilised Al 3the high-density forming core of (Er, Zr) phase, can also reduce the internal stress of large size ingot casting, and thermal distortion and Thermal cracking tendency occur when reducing ingot casting heated fast; The second stage can ensure to eliminate defect in alloy of ingot at 470 DEG C of heating and thermal insulation 24 ~ 48h, and higher temperature can make tiny Al 3(Er, Zr) phase grow into suitable dimension, be of value to stably pinning alloy deformation tissue, carry heavy alloyed thermal stability.
The present invention has following beneficial effect:
Single-stage provided by the present invention and two-step homogenization thermal treatment process, not only can eliminate the defect of As-cast Microstructure, puies forward heavy alloyed hot workability; And Al in alloy can be promoted 3the precipitation of (Er, Zr) heat-resisting disperse phase and growth, contribute to improving the anti-recrystallizing performance of alloy in hot procedure.
Accompanying drawing explanation
Fig. 1 thermal treatment process schematic diagram;
A is Al-Zn-Mg-Cu-Er-Zr alloy single-stage homogenizing heat treatment schematic diagram (scope of single-stage thermal treatment holding temperature T is 450 ~ 490 DEG C, and the scope of soaking time t is 2 ~ 48h)
B is alloy twin-stage homogenizing heat treatment schematic diagram (first step holding temperature T 1be 400 DEG C, soaking time t 1be 6 ~ 10h; Second stage holding temperature T 2be 470 DEG C of soaking times be t 2be 24 ~ 48h)
Fig. 2 is embodiment alloy single-stage Homogenization Treatments changes in hardness curve;
Fig. 3 is embodiment alloy twin-stage Homogenization Treatments conductivity variations curve;
Fig. 4 is a phase area mark change curve in embodiment single-stage Homogenization Treatments alloy;
Fig. 5 heat treated sample transmission electron microscope photo;
A is single-stage 470 DEG C/24h homogenizing heat treated sample transmission electron microscope photo
B is twin-stage 400 DEG C/6h+470 DEG C/24h homogenizing heat treated sample transmission electron microscope photo.
Embodiment
Below in conjunction with the drawings and the specific embodiments, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1: be to a kind of weight percentage: 7.27%Zn, 2.32%Mg, 0.6%Cu, 0.29%Mn, 0.11%Er, 0.13%Zr, impurity <0.2%, surplus be the aluminium alloy of Al be warming up to respectively 450 ~ 490 DEG C insulation 2 ~ 48h after air cooling to room temperature; Carry out 30 groups of experiments (example: 450 DEG C/2h, 450 DEG C/4h, 450 DEG C/8h, 450 DEG C/16h, 450 DEG C/24h, 450 DEG C/48h altogether, all the other temperature classes seemingly), get different heat treatment state sample and carry out Vickers' hardness and the test of corresponding specific conductivity, test result as shown in Figure 2 and Figure 3.Under same temperature, with soaking time increase, increase keeps constant to sample average hardness subsequently, and the specific conductivity of correspondence reduces with the increase of soaking time, keeps stable subsequently; Its hardness of sample after 470 DEG C/24 ~ 48h after single-stage Homogenization Treatments reaches maximum, and corresponding specific conductivity is minimum.
To in embodiment 1 through the sample of different states single-stage Homogenization Treatments, by the once phase in each sample of scanning electron microscopic observation, then add up once shared mutually area fraction (each state gets the mean value of 20 photos).Institute's statistic data as shown in Figure 4, under same temperature, in sample, once the area fraction of phase reduces with the increase of soaking time, keep basicly stable subsequently, the display of whole result after 470 DEG C/24h after single-stage Homogenization Treatments in sample a phase area mark reach Schwellenwert, keep constant subsequently.
Embodiment 2: 400 DEG C are warming up to the alloy cast ingot identical with embodiment 1 and are incubated 6 ~ 10h, after continuing to be warming up to 470 DEG C of insulation 24h subsequently, air cooling is to room temperature; Because two-step homogenization process is also through 470 DEG C/24h process, the as-cast structure defect in its sample and single-stage 470 DEG C/24h process is the same can be eliminated, and only has the difference of disperse phase therebetween; 470 DEG C/24h single-stage homogenizing heat treated sample in 1 in conjunction with the embodiments, respectively by the disperse educt phase Al in transmission electron microscope observing sample two sample 3, as shown in figure 5a and 5b, as can be seen from the figure all there is the Al of Dispersed precipitate in alloy after thermal treatment in the existence of (Er, Zr) particle 3(Er, Zr) particle, and after 400 DEG C/6h+470 DEG C/24h two-step homogenization thermal treatment Al in sample 3(Er, Zr) particle distribution more crypto set, Al in the sample of two states process 3the mean diameter of (Er, Zr) particle is respectively 21.88 and 14.52nm, and these dispersed granules have certain thermotolerance, contributes to improving alloy and grows up in the anti-recrystallizing performance of later stage hot procedure and suppression deformed grains.

Claims (3)

1. the homogenizing heat treatment of Er, Zr combined microalloying Al-Zn-Mg-Cu alloy, wherein alloying constituent: Zn 7.2 ~ 8.2%, Mg 2.0 ~ 3.0%, Cu 0.4 ~ 0.8%, Mn 0.2 ~ 0.5%, Er 0.1 ~ 0.15%, Zr 0.1 ~ 0.15%, inevitable impurity≤0.3, surplus is Er, Zr combined microalloying Al-Zn-Mg-Cu alloy of Al, adopt single-stage homogenizing or two-step homogenization treatment process, it is characterized in that
The thermal treatment of single-stage homogenizing is carried out to this alloy cast ingot: after being incubated 2 ~ 48h after alloy cast ingot is warming up to 450 ~ 490 DEG C respectively, air cooling is to room temperature;
Or two-step homogenization thermal treatment is carried out to this alloy cast ingot: after alloy cast ingot is incubated 6 ~ 10h after being warming up to 400 DEG C, after continuing to be warming up to 470 DEG C of insulation 24 ~ 48h, air cooling is to room temperature.
2. according to the homogenizing heat treatment of a kind of Er, Zr combined microalloying Al-Zn-Mg-Cu of claim 1, it is characterized in that, its alloying constituent is (weight percent): 7.27%Zn, 2.32%Mg, 0.6%Cu, 0.29%Mn, 0.11%Er, 0.13%Zr, impurity <0.2%, and surplus is Al.
3. according to the homogenizing heat treatment of a kind of Er, Zr combined microalloying Al-Zn-Mg-Cu of claim 1, it is characterized in that, single-stage homogenizing heat treating regime is at 470 DEG C of insulation 24 ~ 48h; Two-step homogenization heat treating regime for being warming up to 470 DEG C of insulation 24 ~ 48h again after 400 DEG C of insulation 6 ~ 10h.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711465A (en) * 2015-04-09 2015-06-17 东南大学 Al-Zn-Mg-Cu high-strength aluminum alloy material and preparation method thereof
CN105568190A (en) * 2016-03-16 2016-05-11 北京工业大学 Two-stage aging process of Al-5.6Zn-2.1Mg-1.2Cu-0.1Zr-0.1Er alloy
CN107354412A (en) * 2017-08-09 2017-11-17 中车青岛四方机车车辆股份有限公司 A kind of Al Zn Mg alloy twin-stage homogenization process containing Zr
CN107447144A (en) * 2017-08-10 2017-12-08 辽宁忠大铝业有限公司 A kind of heat-resistant rare earth aluminium alloy and preparation method thereof
CN109666877A (en) * 2019-01-16 2019-04-23 广西大学 A kind of high-temperature processing method with low melting point eutectic tissue aluminium alloy
CN111500951A (en) * 2020-06-03 2020-08-07 西南铝业（集团）有限责任公司 Homogenization heat treatment process of 7050 alloy ingot
CN112095038A (en) * 2020-09-27 2020-12-18 北京工业大学 Method for increasing number of disperse phases in aluminum alloy
CN112695235A (en) * 2020-11-30 2021-04-23 烟台南山学院 Single-stage homogenization heat treatment method for high-alloying Al-Zn-Mg-Cu-Ce alloy
CN113234974A (en) * 2021-05-07 2021-08-10 北京工业大学 Method for reducing thermoplastic deformation resistance of Er microalloyed 7000 series aluminum alloy
CN116219240A (en) * 2023-03-03 2023-06-06 北京工业大学 Ultra-high strength Al-Zn-Mg-Cu alloy compositely added with Er and Zr and preparation process

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CN103243248A (en) * 2013-04-28 2013-08-14 中南大学 Preparation method of extrusion-type aluminum alloy
CN103255327A (en) * 2013-04-27 2013-08-21 北京工业大学 Al-Zn-Mg-Cu-Mn-Zr-Er alloy and preparation technology
CN103710653A (en) * 2013-12-17 2014-04-09 芜湖万润机械有限责任公司 Preparation method of high-strength and high-toughness aluminum alloy profile

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CN101701308A (en) * 2009-11-11 2010-05-05 苏州有色金属研究院有限公司 High-damage tolerance type ultrahigh strength aluminum alloy and preparation method thereof
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711465A (en) * 2015-04-09 2015-06-17 东南大学 Al-Zn-Mg-Cu high-strength aluminum alloy material and preparation method thereof
CN105568190A (en) * 2016-03-16 2016-05-11 北京工业大学 Two-stage aging process of Al-5.6Zn-2.1Mg-1.2Cu-0.1Zr-0.1Er alloy
CN107354412A (en) * 2017-08-09 2017-11-17 中车青岛四方机车车辆股份有限公司 A kind of Al Zn Mg alloy twin-stage homogenization process containing Zr
CN107447144A (en) * 2017-08-10 2017-12-08 辽宁忠大铝业有限公司 A kind of heat-resistant rare earth aluminium alloy and preparation method thereof
CN107447144B (en) * 2017-08-10 2019-07-09 辽宁忠大铝业有限公司 A kind of heat-resistant rare earth aluminium alloy and preparation method thereof
CN109666877B (en) * 2019-01-16 2020-09-08 广西大学 High-temperature treatment method for aluminum alloy with low-melting-point eutectic structure
CN109666877A (en) * 2019-01-16 2019-04-23 广西大学 A kind of high-temperature processing method with low melting point eutectic tissue aluminium alloy
CN111500951A (en) * 2020-06-03 2020-08-07 西南铝业（集团）有限责任公司 Homogenization heat treatment process of 7050 alloy ingot
CN112095038A (en) * 2020-09-27 2020-12-18 北京工业大学 Method for increasing number of disperse phases in aluminum alloy
CN112095038B (en) * 2020-09-27 2022-03-22 北京工业大学 Method for increasing number of disperse phases in aluminum alloy
CN112695235A (en) * 2020-11-30 2021-04-23 烟台南山学院 Single-stage homogenization heat treatment method for high-alloying Al-Zn-Mg-Cu-Ce alloy
CN113234974A (en) * 2021-05-07 2021-08-10 北京工业大学 Method for reducing thermoplastic deformation resistance of Er microalloyed 7000 series aluminum alloy
CN116219240A (en) * 2023-03-03 2023-06-06 北京工业大学 Ultra-high strength Al-Zn-Mg-Cu alloy compositely added with Er and Zr and preparation process

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