CN104451291B - 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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CN104451291B
CN104451291B CN201410676636.8A CN201410676636A CN104451291B CN 104451291 B CN104451291 B CN 104451291B CN 201410676636 A CN201410676636 A CN 201410676636A CN 104451291 B CN104451291 B CN 104451291B
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alloy
heat treatment
treatment process
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homogenizing heat
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CN104451291A (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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Beijing University of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/10Alloys based on aluminium with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/053Changing 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

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 homogenization heat treatment of er, zr combined microalloying al-zn-mg-cu alloy Technique
Technical field
The invention belongs to metal alloy compositions technical field is and in particular to arrive a kind of al-zn-mg-cu-er-zr alloy Single-stage and two-step homogenization Technology for Heating Processing.
Technical background
It is low that al-zn-mg-cu line aluminium alloy has density, and intensity is high, toughness, and hot-workability and decay resistance are preferably etc. Feature, is widely used to the fields such as Aero-Space, shipping industry, communications and transportation, becomes one of primary structural material.But by Higher in al-zn-mg-cu alloying level, process of setting exists serious dendritic segregation, transgranular and Grain Boundary Chemistry composition And Tissue distribution is uneven, these all can seriously drop low-alloyed plasticity, deteriorate hot-working character, make alloy product intensity and Plasticity reduces, and anisotropy and corrosion susceptibility increase.Therefore in order to eliminate ingot structure defect to alloy properties for follow Impact, must reasonably be homogenized heat treatment before ingot casting thermal deformation.
Homogenization heat treatment is an extremely important technical process of alloy preparation and application.At rational homogenization heat Reason can reach following effect: 1), eliminates in alloy cast ingot each element segregation so that each element is uniformly distributed;2), eliminate in alloy Low melting point eutectic phase, puies forward heavy alloyed hot-working character;3), the infusibility phase in nodularization alloy and not melt-phase, improve alloy follow-up Processing characteristics;4), separate out small and dispersed particle, suppression deforming alloy recrystallization and crystal grain are grown up.Therefore for such containing micro- conjunction The al-zn-mg-cu alloy of alloying element er, zr, the homogenizing heat treatment that it is suitable for not only needs to eliminate the one-tenth of alloy cast ingot Point segregation and once phase, are also needed to be heat-treated by homogenization simultaneously, separate out the al of small and dispersed3(er, zr) particle is improving The follow-up performance of alloy.The present invention is on above technical background basis, and accordingly suitable single-stage and twin-stage are uniform to devise this alloy Change Technology for Heating Processing.
Content of the invention
It is an object of the invention to provide being applied to al-zn-mg-cu-er-zr alloy, (the 7xxx system aluminium containing er, zr closes Gold) single-stage homogenization and two-step homogenization Technology for Heating Processing.The casting that provided handling process is not only able to eliminate ingot casting lacks Fall into, improve al-zn-mg-cu-er-zr alloy hot-workability, and thermally-stabilised phase al can be promoted3The analysis of (er, zr) particle Go out, be favorably improved alloy and grow up in the anti-recrystallizing performance of hot procedure and suppression deformed grains.
The present invention provides and is applied to al-zn-mg-cu-er-zr alloy single-stage and two-step homogenization Technology for Heating Processing, its work Skill be suitable for alloy each group be divided into (percentage by weight) 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, the aluminium alloy cast ingot of balance 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%, balance of al.
Provided by the present invention for be applied to al-zn-mg-cu-er-zr alloy single-stage and two-step homogenization heat treatment work Skill, its technique comprises the following steps:
1), single-stage homogenization heat treatment is: alloy cast ingot is incubated 2~48h after being warming up to 450~490 DEG C respectively;It optimizes Single-stage homogenization heat treating regime is to be air cooled to room temperature after 470 DEG C of insulation 24~48h, as shown in Figure 1a.
2), two-step homogenization is heat-treated and is: alloy cast ingot is warming up to 400 DEG C of insulation 6~10h, continues thereafter with and is warming up to 470 DEG C insulation 24~48h after be air cooled 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 so that alloying component distribution is equal Even, eliminate the infusibility phase in low melting point phase the nodularization alloy in alloy, it is possible to increase the follow-up hot-working character of alloy, with When this single-stage Homogenization Treatments technique can separate out the al of small and dispersed3(er, zr) particle.
Two-step homogenization handling process of the present invention is further perfect on the basis of this single stage process, and its first order exists 400 DEG C of heating and thermal insulations, are conducive to the precipitation of the microalloy element such as er, zr in alloy, promote thermally-stabilised al3(er, zr) phase High density forming core, can also reduce the internal stress of large scale ingot casting, reduce and thermal deformation and Thermal cracking occur during ingot casting heated fast Tendency;The second level ensure that defect in elimination alloy of ingot in 470 DEG C of heating and thermal insulation 24~48h, and higher temperature can Make tiny al3(er, zr) phase grow into suitable dimension, be beneficial to stably pinning alloy deformation tissue, carry heavy alloyed Thermal stability.
The present invention has a following beneficial effect:
Single-stage provided by the present invention and two-step homogenization Technology for Heating Processing, not only can eliminate lacking of As-cast Microstructure Fall into, put forward heavy alloyed hot-working character;And al in alloy can be promoted3The precipitation of (er, zr) heat-resisting disperse phase and growth, have Help improve the anti-recrystallizing performance in hot procedure for the alloy.
Brief description
Fig. 1 Technology for Heating Processing schematic diagram;
A is that (single-stage is heat-treated holding temperature to al-zn-mg-cu-er-zr alloy single-stage homogenizing heat treatment schematic diagram The scope of t is 450~490 DEG C, and the scope of temperature retention time t is 2~48h)
B is alloy twin-stage homogenizing heat treatment schematic diagram (first order holding temperature t1For 400 DEG C, temperature retention time t1For 6~10h;Second level holding temperature t2It is t for 470 DEG C of temperature retention times2For 24~48h)
Fig. 2 is embodiment alloy single-stage Homogenization Treatments firmness change curve;
Fig. 3 is embodiment alloy twin-stage Homogenization Treatments conductivity variations curve;
Fig. 4 is a phase area fraction change curve in embodiment single-stage Homogenization Treatments alloy;
Fig. 5 heat treated sample transmission electron microscope photo;
A is that 470 DEG C/24h of single-stage homogenizes heat treated sample transmission electron microscope photo
B is that 400 DEG C/6h+470 DEG C/24h of twin-stage homogenizes heat treated sample transmission electron microscope photo.
Specific 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 reality Apply example.
A kind of embodiment 1: be to weight percentage: 7.27%zn, 2.32%mg, 0.6%cu, 0.29%mn, 0.11%er, 0.13%zr, impurity < 0.2%, after the aluminium alloy of balance of al is warming up to 450~490 DEG C of insulation 2~48h respectively It is air cooled to room temperature;Carried out altogether 30 groups experiment (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, remaining temperature is similar to), take different heat treatment state sample to carry out Vickers hardness and corresponding electrical conductivity and survey Examination, test result is as shown in Figure 2 and Figure 3.Under same temperature, sample average hardness increases with temperature retention time and increases and subsequently keep permanent Fixed, and corresponding electrical conductivity reduces with the increase of temperature retention time, subsequently keeps stable;Single-stage after 470 DEG C/24~48h Its hardness of sample after Homogenization Treatments reaches maximum, and corresponding electrical conductivity is minimum.
To the sample through different conditions single-stage Homogenization Treatments in embodiment 1, by each sample of scanning electron microscopic observation In once phase, then count once the area fraction shared by phase (each state takes the mean value of 20 photos).Institute's statistical number According to as shown in figure 4, once the area fraction of phase reduces with the increase of temperature retention time in sample under same temperature, subsequently keep base Originally stably, in sample after whole result shows single-stage Homogenization Treatments after 470 DEG C/24h, a phase area fraction reaches Low value, subsequently keeps constant.
Embodiment 2: alloy cast ingot same as Example 1 is warming up to 400 DEG C of insulation 6~10h, continues thereafter with and be warming up to It is air cooled to room temperature after 470 DEG C of insulation 24h;Also pass through 470 DEG C/24h process, the as cast condition in its sample because two-step homogenization is processed 470 DEG C/24h of tissue defects and single-stage can be eliminated as processing, therebetween the difference of only disperse phase;In conjunction with the embodiments 1 In 470 DEG C/24h single-stage homogenization heat treated sample, respectively pass through transmission electron microscope observing sample two sample in disperse educt phase al3The existence of (er, zr) particle, as shown in figure 5a and 5b, all occurs in that in alloy after being as can be seen from the figure heat-treated The al of Dispersed precipitate3(er, zr) particle, and al in sample after the heat treatment of 400 DEG C/6h+470 DEG C/24h two-step homogenization3 (er, zr) particle is distributed more crypto set, al in the sample that two states are processed3The average diameter of (er, zr) particle is respectively 21.88 and 14.52nm, these dispersed granules have certain heat resistance, are favorably improved alloy in later stage hot procedure Anti-recrystallizing performance and suppression deformed grains are grown up.

Claims (2)

1. a kind of homogenizing heat treatment of er, zr combined microalloying al-zn-mg-cu alloy, wherein alloying component: 7.27%zn, 2.32%mg, 0.6%cu, 0.29%mn, 0.11%er, 0.13%zr, impurity < 0.2%, the er of balance of al, Zr combined microalloying al-zn-mg-cu alloy, using single-stage homogenization or two-step homogenization handling process it is characterised in that
This alloy cast ingot is carried out with single-stage homogenization heat treatment: alloy cast ingot is warming up to respectively after 450~490 DEG C insulation 2~ It is air cooled to room temperature after 48h;
Or this alloy cast ingot is carried out with two-step homogenization heat treatment: by alloy cast ingot in being warming up to after insulation 6~10h after 400 DEG C, It is air cooled to room temperature after being continuously heating to 470 DEG C of insulation 24~48h.
2. according to a kind of homogenizing heat treatment of er, zr combined microalloying al-zn-mg-cu alloy of claim 1, It is characterized in that, single-stage homogenization heat treating regime is to be incubated 24~48h at 470 DEG C;Two-step homogenization heat treating regime be It is warming up to 470 DEG C of insulation 24~48h again after 400 DEG C of insulation 6~10h.
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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
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
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
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
CN113234974B (en) * 2021-05-07 2022-07-01 北京工业大学 Method for reducing thermoplastic deformation resistance of Er microalloyed 7000 series aluminum alloy

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