CN102534324A - High-zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment technique - Google Patents

High-zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment technique Download PDF

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CN102534324A
CN102534324A CN201210048787XA CN201210048787A CN102534324A CN 102534324 A CN102534324 A CN 102534324A CN 201210048787X A CN201210048787X A CN 201210048787XA CN 201210048787 A CN201210048787 A CN 201210048787A CN 102534324 A CN102534324 A CN 102534324A
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alloy
heating
stage
timeliness
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CN102534324B (en
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陈子勇
张瑞岩
冉凡青
聂祚仁
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention relates to a high-zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment technique, belonging to the technical field of metal alloys. The technique comprises the following steps: after carrying out solution quenching on aluminum alloy, which comprising 10.0-11.5 wt% of Zn, 1.6-2.0 wt% of Mg, 1.4-2.0 wt% of Cu, 0.08-0.15 wt% of Zr, 0.06-0.15 wt% of Er and the balance of Al and inevitable impurities, heating at 130-140 DEG C for 2-6 hours, and then heating at 115-125 DEG C for 6-10 hours; carrying out high temperature short time aging; and heating the alloy subjected to double-stage aging treatment at 170-200 DEG C for 5-60 minutes. On the premise of keeping the alloy strength unchanged or slightly decreased, the invention enhances the toughness, shortens the heat treatment time and lowers the energy consumption.

Description

A kind of high zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment process
Technical field
The invention belongs to field of metal alloy technology, is the comprehensive accurate thermal treatment process of the specific high zinc high strength alumin ium alloy of a kind of raising.
Background technology
The Al-Zn-Mg-Cu alloy belongs to ultra-high-strength aluminum alloy, is heat-treatable strengthened alloy, has higher specific tenacity; Be widely used in aerospace field; But because under the peak value timeliness state, stress corrosion resistant ability and fracture toughness property are all poor, have limited its widespread use.Therefore, optimize the good alloy of alloying constituent and thermal treatment process acquisition over-all properties is the target of the common pursuit of vast investigation of materials work always.
The following several method of the main at present employing of Al-Zn-Mg-Cu alloy aging technology: single-stage aging, twin-stage overaging and regression and re-ageing.
1) single-stage aging is the peak value timeliness, and its deposition sequence is in the transitory stage of GP district to η ' phase, and the GP district that intracrystalline is mainly distributing trickle and the η ' of a spot of half coherence grow up and the volume(tric)fraction increase with the prolongation precipitate of timeliness time mutually gradually; Simultaneously separate out successive η phase on the crystal boundary, crystal boundary does not have deposition, and to separate out band (PFZ) not obvious.Though but alloy strength peaking (T6) after the complete timeliness, gravitation-resistant corrosive power and toughness are all poor.
2) the twin-stage overaging is to be master's timeliness to improve the gravitation-resistant corrosive power; The first step timeliness of twin-stage overaging is the low temperature preageing; Be equivalent to the timeliness nucleation stage, intracrystalline forms a large amount of GP districts and few η ' mutually, and second stage timeliness is the long time aging of high temperature; Those can the preferential nucleation in GP district of stable existence be converted into η ' phase and grow up gradually under the high-temperature aging temperature, original η ' phase also grow up gradually simultaneously part η ' in opposite directions η change mutually.Mainly form equally distributed η ' phase and η mutually at intracrystalline; The alligatoring of prolongation intracrystalline precipitated phase, particle spacing with the timeliness time increase; It on high-angle boundary more stable η phase; The crystal boundary precipitated phase is discontinuously arranged, has improved the stress corrosion resistant ability and the toughness of alloy, but wants certain intensity of expendable material.
3) regression and re-ageing technology (RRA) comprises three phases: the first step is a single-stage peak value timeliness, makes alloy reach the T6 state; Second stage timeliness is the high temperature regression treatment, makes the dissolving of alloy intracrystalline strengthening phase, and grain boundary precipitate is separated out mutually; The third stage carries out a T6 again and handles.But the RRA treatment process standard that U.S. Alcoa company in 1989 runs after fame and registered first industrial application with T77.After as a rule accomplishing three grades of timeliness, because aging time is long, need carries out twice T6 and handle, energy consumption is higher, is unfavorable for industrial application.
Summary of the invention
It is high to the present invention is directed to the strong Al-Zn-Mg-Cu alloy strength of current high zinc superelevation, and relatively poor this shortcoming of toughness is through using a kind of novel thermal process technology; Make alloy remain unchanged or have slightly under the situation of decline in intensity; The realization flexible improves, and has reduced heat treatment time simultaneously, cuts down the consumption of energy.
Technical scheme of the present invention is: carry out two-stage time effect earlier, guarantee that the supersaturation solute atoms after solution hardening can be with GP district and η ' (MgZn mutually 2) form exist, make alloy reach higher timeliness intensity, then carry out the high temperature, short time timeliness again, the bigger GP district that intracrystalline has been separated out all is converted into η ' phase (MgZn 2), grain boundary precipitate phase η (MgZn 2) nodularization takes place, be interrupted distribution, thereby realize improving alloy flexible purpose.Can make alloy remain unchanged or have slightly under the situation of decline through above ageing treatment, realize that flexible significantly improves, enlarge the range of application of alloy, effectively the shortening heat treatment time, cut down the consumption of energy in intensity.
Operational path of the present invention:
1) two-stage time effect after solution hardening, heated 6 hours~10 hours at 115 ℃~125 ℃ 130 ℃~140 ℃ heating in 2 hours~6 hours subsequently.The first step 130 ℃~140 ℃ heating 2 hours~6 little time aging can make after solution hardening the supersaturation solute atoms with the form in GP district faster homogeneous nucleation can separate out a spot of η ' (MgZn mutually simultaneously with growing up 2), 115 ℃~125 ℃ heating 6 hours~10 hours, the GP district was gradually to η ' phase (MgZn subsequently 2) original η ' phase (MgZn of conversion while 2) grow up, the intensity that makes alloy near or a little less than peak value timeliness intensity.
2) high temperature, short time timeliness, the alloy that will pass through the two-stage time effect processing was heating 5 minutes~60 minutes at 170 ℃~200 ℃, and the GP district that the alloy intracrystalline has been separated out all is converted into η ' phase (MgZn 2), crystal boundary balance precipitated phase η (MgZn 2) the generation nodularization becomes interrupted distribution by continuous distribution, thereby realization improves alloy flexible purpose.
Solution hardening refers to alloy through 470 ℃ of insulations solution hardening in 3 hours in the above-mentioned steps (1).
The alloying constituent that the present invention was suitable for is Zn:10.0%~11.5wt%; Mg:1.6%~2.0wt%; Cu:1.4%~2.0wt%; Zr:0.08%~0.15wt%; Er:0.06~0.15wt%, surplus is Al and some other inevitable impurity.
Advantage of the present invention and positively effect:
1) separate out the η ' phase of small and dispersed through the alloy intracrystalline after the present invention's processing, the crystal boundary precipitated phase intermittently distributes;
2) simple to operate, shortened aging time greatly, reduce the thermal treatment energy consumption, help energy-saving and emission-reduction in the industrial production;
3) alloy is being kept the high-intensity while, improve the toughness of alloy.
Description of drawings
Fig. 1 alloy is at 90 ℃~165 ℃, and the time is 0.5 hour~72 hours changes in hardness law curve;
Fig. 2 is that alloy is after 8 hours (two-stage time effect) heated in 4 hours+120 ℃ of 135 ℃ of heating, in the age hardening curves of 170 ℃ of heating 5 minutes~240 minutes (high temperature, short time timeliness);
Fig. 3 is that alloy is after 8 hours (two-stage time effect) heated in 4 hours+120 ℃ of 135 ℃ of heating, in the age hardening curves of 180 ℃ of heating 5 minutes~240 minutes (high temperature, short time timeliness);
Fig. 4 is that alloy is after 8 hours (two-stage time effect) heated in 4 hours+120 ℃ of 135 ℃ of heating, in the age hardening curves of 190 ℃ of heating 5 minutes~240 minutes (high temperature, short time timeliness);
Fig. 5 is that alloy is after 8 hours (two-stage time effect) heated in 4 hours+120 ℃ of 135 ℃ of heating, in the age hardening curves of 200 ℃ of heating 5 minutes~240 minutes (high temperature, short time timeliness);
Fig. 6 is the grain boundary precipitate phase character figure of alloy after 120 ℃ of heating were handled in 24 hours;
Fig. 7 is the intracrystalline precipitated phase characteristic pattern of alloy after aging technique of the present invention is handled;
Fig. 8 is the grain boundary precipitate phase character figure of alloy after aging technique of the present invention is handled
The practical implementation method
Alloy composition is that the extruding attitude alloy (extrusion ratio is 15.4: 1) of Al-10.0Zn-1.9Mg-1.7Cu-0.12Zr-0.06Er (mass percent) carries out 470 ℃ of solution treatment in 3 hours with alloy; Shrend is carried out the ageing treatment of following embodiment subsequently to room temperature.
Comparative Examples 1
1) alloy is carried out single-stage aging and handle, the single-stage aging temperature is 90 ℃~165 ℃, and the time is 0.5 hour~72 hours, gets the sample test hardness of different heat treatment state, draws out the hardness curve (see figure 1).Can be found out that by Fig. 1 alloy has very significantly aging hardening behavior, at the timeliness initial stage, hardness rises very obvious.Curve changes in hardness trend is basic identical, has all experienced one and has risen to the process that peak value slowly descends subsequently earlier.Alloy reaches peak value in 24 hours hardness of 120 ℃ of timeliness.
2) choosing near the single-stage aging peak point (120 ℃ timeliness 24 hours) the state sample carries out the Mechanics Performance Testing result and sees table 1.The variation of alloy strength and hardness curve basically identical.Alloy was obtained peak strength in 24 hours at 120 ℃, and this moment, the fracture toughness property of alloy was 31.4MPa 1/2
The mechanical property of table 1 alloy after 120 ℃ of single-stage agings are handled
The timeliness state σ b/MPa σ 0.2/MPa δ 5/%
120℃/16h 738 700 10.3
120℃/20h 735 700 11
120℃/24h 763 733 9.3
120℃/28h 735 705 10.3
Comparative Examples 2
1) alloy being carried out two-stage time effect handles: first step ageing treatment be 135 ℃ 2 hours~6 hours, second stage ageing treatment be 120 ℃ 8 hours.Choose different heat treatment state sample and carry out hardness test, the result sees table 2.It is thus clear that, optimum first step ageing treatment be 135 ℃ 4 hours.
The hardness of table 2 alloy after 135 ℃ of 2 hours~6 hours+120 ℃ 8 hours ageing treatment
The timeliness state Hardness/HV
135℃/2h+120℃/8h 201.1
135℃/4h+120℃/8h 206.7
135℃/6h+120℃/8h 202.3
2) alloy being carried out two-stage time effect handles: first step ageing treatment be 135 ℃ 4 hours, second stage ageing treatment be 120 ℃ 6 hours~10 hours.Choose different heat treatment state sample and carry out hardness test, the result sees table 3.It is thus clear that, optimum second stage ageing treatment be 120 ℃ 8 hours.So optimized twin-stage technology is 4 hours+120 ℃ heating of 135 ℃ of heating 8 hours, this moment, tensile strength of alloys was that 749MPa, ys 716Mpa, unit elongation are 10.1%, fracture toughness property 30.3MPa 1/2
The hardness of table 3 alloy after 135 ℃ of 4 hours+120 ℃ 6 hours~10 hours ageing treatment
The timeliness state Hardness/HV
135℃/4h+120℃/6h 202.5
135℃/4h+120℃/8h 206.7
135℃/4h+120℃/10h 205.2
Embodiment 3
The two-stage time effect process is referring to Comparative Examples 2, and the alloy after preferably will handling through 4 hours+120 ℃ heating of 135 ℃ of heating 8 hours (two-stage time effect) heats 5 minutes~60 minutes (high temperature, short time timeliness) at 170 ℃~200 ℃, and age hardening curves is seen Fig. 2~Fig. 5.Can find out that under different high-temperature temperatures the Vickers' hardness of alloy all the characteristics of dullness decline again that afterwards rise occur reducing earlier along with the prolongation of time, and along with the increase of high-temperature temperature, shift to an earlier date the time that valley and peak value appear in alloy Vickers' hardness curve to some extent.Table 4 explanation alloy will have better comprehensive performance in 190 ℃ of heating 15 minutes (high temperature, short time timeliness) after 4 hours+120 ℃ heating of 135 ℃ of heating 8 hours (two-stage time effect) are handled.
The hardness of table 4 alloy after 135 ℃ 4 hours+120 ℃ 8 hours+190 ℃ 5~20 minutes ageing treatment
Three grades of aging techniques σ b/MPa σ 0.2/MPa δ 5/% KIC/MPa 1/2
135℃/4h+120℃/8h+190℃/5min 736 730 9.0 36.2
135℃/4h+120℃/8h+190℃/10min 718 680 12.0 35.5
135℃/4h+120℃/8h+190℃/15min 725 708 13.0 38.0.
135℃/4h+120℃/8h+190℃/20min 731 676 10.7 32.2
Embodiment 4
After will passing through 4 hours+120 ℃ heating of 135 ℃ of heating of aging technique of the present invention (two-stage time effect) processing in 8 hours; Tensile strength, unit elongation, the fracture toughness property of alloy property of handling in 190 ℃ of heating 15 minutes (high temperature, short time timeliness) and single-stage aging (120 ℃ 24 hours), two-stage time effect (135 ℃ 4 hours+120 ℃ 8 hours) compare, and the result sees table 5.
The different aging techniques of table 5 are handled the performance of back alloy
Aging technique σ b/MPa σ 0.2/MPa δ 5/% KIC/MPa 1/2
120℃/24h 763 733 9.3 31.4
135℃/4h+120℃/8h 749 716 10.1 30.3
135℃/4h+120℃/8h+190℃/15min 725 708 13.0 38.0
Can find out that from table 5 alloy property after thermal treatment process of the present invention is handled is except that tensile strength and ys slightly descend than single-stage aging and two-stage time effect state, unit elongation and fracture toughness property all are higher than single-stage aging, two-stage time effect.This technology has shortened aging time simultaneously, has reduced energy consumption.
By through alloy intracrystalline precipitated phase and grain boundary precipitate microstructure characteristic figure (Fig. 7 mutually after 135 ℃ of the embodiment of the invention 4/4h+120 ℃/8h+190 ℃/15min thermal treatment; 8) can find out that alloy inside separated out the tiny and uniform precipitated phase, grain boundary precipitate intermittently distributes mutually.The grain boundary precipitate phase character figure (Fig. 6) of comparative alloy after 120 ℃ of heating were handled (T6 processing) in 24 hours; Can find out when the alloy after the thermal treatment of the present invention is keeping T6 state intracrystalline precipitated phase to distribute; The continuous distribution of grain boundary precipitate phase that interrupted T6; Thereby keeping the high-intensity while, improving the toughness of alloy.

Claims (3)

1. one kind high zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment process; Al alloy component is Zn:10.0wt%~11.5wt%, Mg:1.6wt%~2.0wt%, Cu:1.4wt%~2.0wt%, Zr:0.08wt%~0.15wt%, Er:0.06wt%~0.15wt%; Surplus is Al and some other inevitable impurity; It is characterized in that, may further comprise the steps:
1) two-stage time effect after solution hardening, heated 6 hours~10 hours at 115 ℃~125 ℃ 130 ℃~140 ℃ heating in 2 hours~6 hours subsequently;
2) high temperature, short time timeliness, the alloy that will pass through the two-stage time effect processing was heating 5 minutes~60 minutes at 170 ℃~200 ℃.
2. according to the technology of its claim 1, it is characterized in that two-stage time effect is that the high temperature, short time timeliness be to heat 15 minutes at 190 ℃ in 135 ℃ of heating 4 hours, 120 ℃ of heating 8 hours then.
3. according to the technology of its claim 1, it is characterized in that solution hardening refers to alloy through 470 ℃ of insulations solution hardening in 3 hours in the step (1).
CN201210048787.XA 2012-02-28 2012-02-28 High-zinc high-strength Al-Zn-Mg-Cu aluminum alloy heat treatment technique Expired - Fee Related CN102534324B (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103993211A (en) * 2014-06-06 2014-08-20 江苏大学 720-750MPa super strength non-rapid-solidification aluminum alloy and preparation method thereof
CN104357776A (en) * 2014-10-24 2015-02-18 陈帆 Processing method of 2014 aluminum alloy plate
CN104357777A (en) * 2014-10-24 2015-02-18 陈帆 Processing method of 2A01 aluminum alloy plate
CN104372268A (en) * 2014-10-24 2015-02-25 陈帆 Processing method of 2011 aluminum alloy plate
CN112410690A (en) * 2020-11-20 2021-02-26 郭洋 Aging treatment method for improving mechanical property of Al-Zn-Mg-Cu alloy
CN114774747A (en) * 2022-05-12 2022-07-22 广东豪美新材股份有限公司 High-strength 7000 series aluminum alloy section and processing and preparation method thereof
CN115053008A (en) * 2020-02-04 2022-09-13 爱信轻金属株式会社 Method for manufacturing high-strength aluminum alloy extruded material

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WO2001048259A1 (en) * 1999-12-23 2001-07-05 Commonwealth Scientific And Industrial Research Organisation Heat treatment of age-hardenable aluminium alloys
CN102011073A (en) * 2010-12-03 2011-04-13 北京工业大学 Aging process for improving strengthening and toughening levels of Al-Zn-Mg-Cu alloy
CN102011037A (en) * 2010-12-10 2011-04-13 北京工业大学 Rare earth Er microalloyed Al-Zn-Mg-Cu alloy and preparation method thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103993211A (en) * 2014-06-06 2014-08-20 江苏大学 720-750MPa super strength non-rapid-solidification aluminum alloy and preparation method thereof
CN103993211B (en) * 2014-06-06 2016-03-09 江苏大学 720-750MPa superstrength non-rapid solidifies aluminium alloy and preparation method thereof
CN104357776A (en) * 2014-10-24 2015-02-18 陈帆 Processing method of 2014 aluminum alloy plate
CN104357777A (en) * 2014-10-24 2015-02-18 陈帆 Processing method of 2A01 aluminum alloy plate
CN104372268A (en) * 2014-10-24 2015-02-25 陈帆 Processing method of 2011 aluminum alloy plate
CN115053008A (en) * 2020-02-04 2022-09-13 爱信轻金属株式会社 Method for manufacturing high-strength aluminum alloy extruded material
CN112410690A (en) * 2020-11-20 2021-02-26 郭洋 Aging treatment method for improving mechanical property of Al-Zn-Mg-Cu alloy
CN114774747A (en) * 2022-05-12 2022-07-22 广东豪美新材股份有限公司 High-strength 7000 series aluminum alloy section and processing and preparation method thereof

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