CN110157962A - A kind of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy and preparation method - Google Patents

A kind of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy and preparation method Download PDF

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CN110157962A
CN110157962A CN201910384704.6A CN201910384704A CN110157962A CN 110157962 A CN110157962 A CN 110157962A CN 201910384704 A CN201910384704 A CN 201910384704A CN 110157962 A CN110157962 A CN 110157962A
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aluminum alloy
strength aluminum
alloy
aluminium alloy
surplus
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CN110157962B (en
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李春梅
程南璞
蒋显全
唐剑锋
郭宁
李路
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Southwest University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • 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 present invention relates to the regulations of the composition of the tough aluminum alloy materials of the strong superelevation of aerospace superelevation, process and heat treatment technique, particular for the aluminium alloy requirement of high-strength and high ductility high-hardenability needed for aerospace, it proposes a kind of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy and preparation method, belongs to technical field of aluminum alloy technology.The aluminium alloy each component and its mass percent are as follows: Zn 7.2~9.5%, Mg 1.2~2.5%, Cu 1.3~1.9%, Zr 0.08~0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.Compared with existing such aluminium alloy, it is not necessarily to improve cost the comprehensive performance, it can be achieved that strength and toughness and high-hardenability by technical solution of the present invention;It is discharged in preparation and heat treatment process of the invention without waste water and gas, pollution-free, the requirement for equipment is lower, is conducive to industrialized production and popularization and application.

Description

A kind of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy and preparation method
Technical field
The present invention relates to the regulations of the composition of the tough aluminum alloy materials of the strong superelevation of aerospace superelevation, process and heat treatment work Skill proposes a kind of Al-Zn-Mg-Cu system particular for the aluminium alloy requirement of high-strength and high ductility high-hardenability needed for aerospace Ultra-high-strength aluminum alloy and preparation method, belong to technical field of aluminum alloy technology.
Background technique
Al-Zn-Mg-Cu aluminum alloy is due to high specific strength, specific modulus, good conductive and heat-conductive corrosion resistance, excellent The features such as good cutting ability, it is widely used in aerospace, automobile, machine-building, ship, chemical industry and civilian work Industry.With Global Aerospace cause broad development, the requirement to high-strength aluminum alloy is also higher and higher.But intensity improves general Alloy plasticity can be caused to decline, to obtain the alloy of high-strength and high-plasticity, it is necessary to the contradiction of strength and toughness restriction is solved, so that It is comprehensive to can be promoted.Meanwhile to meet the needs of big part aerospace material, it is necessary to assure aluminium alloy is in high-strength and high ductility There is good harden ability simultaneously, i.e., hardening constituent the process of precipitation cannot be too sensitive to temperature gradient.
The optimization and improvement of aluminium alloy capability are mainly realized by five kinds of approach: first is that main alloying element regulates and controls, realization pair The control of hardening constituent classification, so as to adjust alloy macroscopic property;Second is that microalloy element adds, pass through the preferential analysis of microalloy phase Out, refinement and reinforced aluminium alloy matrix;Third is that molding mode, by precipitation in situ, compound implantation or fast cold forming to obtain spy The improvement of qualitative energy;Fourth is that shaping, refining crystal grain using deformation and forming dislocation pinning, improve alloy property;Fifth is that hot Treatment process improves the size and distribution of hardening constituent by the diffusion of precipitated phase, back dissolving and precipitation, thus optimize microstructure, Improve alloy property.
Currently, the aluminium alloy composition regulation reported both at home and abroad, which mostly uses addition rare earth element to form disperse phase, comes pinning position Wrong, sub boundary and crystal boundary play the role of dispersion-strengtherning, substructure reinforcing, realize the promotion of performance.But rare earth is expensive, It is not appropriate for being widely used in structural material.And heat treatment process, including homogenization, solid solution and timeliness, then pass through single-stage or double Grade strengthens homogenization and solid solution, and peak value timeliness is combined to complete, and is difficult to realize the two-win of strength and toughness.
It is specific that literature survey shows that the main alloying element regulation to Al-Zn-Mg-Cu aluminum alloy is heat-treated with deep cooling The not disclosed report of technique.
Summary of the invention
Big block part aluminium alloy needed for the present invention is directed to aerospace proposes that a kind of strong aluminium of Al-Zn-Mg-Cu system superelevation closes Gold and preparation method thereof, the aluminium alloy optimize the reinforcing facies type of aluminium alloy by adjusting main alloying element, guarantee alloy While strength and toughness, there is high harden ability;And the multistage by developing double deep cooling insertions in prior heat treatment process Heat treatment process adjusts the distribution of hardening constituent, promotes matrix metastable state Dispersed precipitate density, and regulation crystal boundary stable phase is interrupted Distribution and pollution freemetallurgy, to realize the promotion of superelevation super tenacity aluminum alloy comprehensive performance by force.
The technical solution adopted by the present invention are as follows:
A kind of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy, each component and its mass percent are as follows: Zn 7.2~9.5%, Mg 1.2~2.5%, Cu 1.3~1.9%, Zr 0.08~0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
Cu constituent content in 1.3~1.9% ranges, is limited S phase (Al by the present invention2CuMg the maximum volume) being mutually precipitated Score;By Mg constituent content be arranged in 1.2~2.5% ranges, regulate and control alloy in hardening constituent volume fraction, meet intensity and The demand of toughness;By the regulation of Zn constituent content in 7.2~9.5% ranges, η phase (MgZn is improved2) volume fraction, and Mg element is consumed in precipitation process, inhibits S phase (Al2CuMg formation).
The present invention also proposes the preparation method of more than one aluminium alloys, comprising the following steps:
(1) it is handled by alloy composition through ingredient, melting (i.e. alloying), cleaning molten and crystal grain refinement, cast molding shape It is air-cooled at ingot casting, demoulding.Smelting temperature is controlled at 750-770 DEG C, if temperature is excessively high, the scaling loss of alloy will be excessive.Cleaning molten Using N2Refining, reaches low hydrogen content, avoids hydrogen-induced fracture.To accomplish " three is pure " in entire process flow: first is that Fe, The impurity contents such as Si are low;Second is that oxide Al2O3Equal oxide inclusions are low;Third is that it is hydrogeneous be mingled with it is low.The serious shadow of the meeting of generation is avoided as far as possible Ring (Fe, Cr) SiAl of the fracture toughness of alloy12、(Fe,Mn,Cu)Al6、Cu2FeAl7、Mg2The impurity phases oversize grain such as Si.
(2) to step (1) ingot casting use compound Homogenization Treatments: 430 DEG C heat preservation 46 hours after be warming up to 467 DEG C of heat preservations Then 4h comes out of the stove air-cooled.
(3) hot extrusion is carried out to the ingot casting after step (2) compound Homogenization Treatments.When extruding, metal temperature be 400~ 440 DEG C, heating time 2h;Extrusion cylinder, mold, cushion temperature be 440~480 DEG C, heating time 12h.
(4) subzero treatment is carried out to the resulting extrusion of step (3): keeps the temperature 36 hours at -197 DEG C.
(5) carry out three-stage solution to the resulting subzero treatment sample of step (4): 450~470 DEG C keep the temperature 20~40 minutes After be warming up to 470~480 DEG C of heat preservations and be warming up within 20 minutes 480~490 DEG C again and keep the temperature 20 minutes, then water quenching or oil quenching.
(6) to the resulting solid solution sample of step (5) carry out two-stage time effect: 120~135 DEG C heat preservation 16 hours after be warming up to 190 DEG C keep the temperature 10 minutes.
(7) subzero treatment is carried out to step (6) resulting aging samples again: keeping the temperature 36 hours at -197 DEG C.
The present invention is based on following principles:
Theoretical and Experimental Study shows that the main hardening constituent of Al-Zn-Mg-Cu aluminum alloy is η phase (MgZn2), while easily Form S phase (Al2) and θ phase (Al CuMg2Cu).Wherein, S phase (Al2) and η phase (MgZn CuMg2) Precipitation Temperature it is close.And η phase (MgZn2) compared with S phase (Al2) and θ phase (Al CuMg2Cu) there is bigger TiFe_xM_y alloy, from thermodynamic (al) angle η phase (MgZn2) analysis Driving force is bigger out, therefore in casting process, η phase (MgZn2) with S phase (Al2CuMg) competitive precipitation.Meanwhile η phase (MgZn2) compared with S phase (Al2) and θ phase (Al CuMg2Cu) there is smaller combination energy, thus easily decomposes and diffusion.And heating power It learns studies have shown that η phase (MgZn2) the no S phase (Al of precipitation2) and θ phase (Al CuMg2Cu the variation for) depending on temperature gradient, because This is not strong to the sensibility of temperature in heat treatment process, especially quenching process, and determines it and massive material may be implemented High-hardenability.The present invention proposes the reinforcing facies type for optimizing aluminium alloy by adjusting main alloying element, guarantees alloy strength While with toughness, there is high harden ability.In order to guarantee that material has good solid solubility and harden ability, composition design needs to protect Demonstrate,prove η phase (MgZn2) abundant precipitation, and control S phase (Al2CuMg volume fraction).Low content of Cu suitably drops, and it is crisp to control Property indissoluble S phase (Al2) and θ phase (Al CuMg2Cu precipitation).And on the basis of Mg content, high Zn content is mentioned, guarantees η phase (MgZn2) volume fraction, and in precipitation process consume Mg element, inhibit S phase (Al2CuMg formation).
Alloy composition is designed according to corrosion resistance and strength character demand, determines Cu constituent content in 1.3~1.9% ranges It is interior, limit S phase (Al2CuMg the maximum volume score) being mutually precipitated.Based on Al2Atomic ratio A in CuMg phaseMg:ACu=1:1, should Two kinds of element mass ratio M in phaseMg:MCu=1:2.7, if Cu element is with Al2CuMg phase is precipitated, then Mg content needed for the phase Within the scope of 0.5-0.7%.Based on MgZn2Atomic ratio A in phaseMg:AZnOn the basis of=1:2, the quality of two kinds of elements in the phase Compare MMg:MZn=1:5.4.If the Mg of 0.5-0.7% is in casting process with Al2CuMg phase is precipitated, while considering Mg melting loss of elements 0.1%, then MgZn2The also surplus 0.6-1.7% of Mg content in phase, forms MgZn2Zn constituent content needed for phase 3.2~ In 9.0% range.The regulation of Zn constituent content is in 7.2~9.5% ranges in the present invention, to improve η phase (MgZn2) volume point Number, and Mg element is consumed in precipitation process, inhibit S phase (Al2CuMg formation).
In addition, adjusting hardening constituent by the multistage heat treatment process for developing double deep cooling insertions in prior heat treatment process Distribution, when hardening constituent being allowed to be precipitated again after solid solution, promoted matrix metastable state Dispersed precipitate density, crystal boundary is with stable phase Discontinuously distribution, to realize the promotion of superelevation super tenacity aluminum alloy comprehensive performance by force, double the multistage of deep coolings insertion are heat-treated Technique is as follows: the first step, is deep cooling after deformation, it is therefore an objective to be realized and be replied using deformation residual stress and shrinkage stress, refinement is brilliant Matrix energy is reduced while grain, is reduced the driving force that solid solution process forming core is grown up, is reached grain refinement effect;Second step, three Grade solid solution, combines when low temperature is long with high temperature, short time, the η phase (MgZn for first allowing easily decomposition to be spread2) back dissolving, then improve solid solution temperature Degree avoids realizing S phase (Al as far as possible while burning2) and θ phase (Al CuMg2Cu solid solution) finally carries out third level solid solution, Temperature is improved to obtain high supersaturated solid solution, provides good matrix for Precipitation;Third step carries out two-stage time effect, When low temperature is long and high temperature, short time, the disperse educt in the area GP and η ' phase is realized when low temperature is long, is avoided to η phase (MgZn2) transformation, High temperature, short time ageing treatment is carried out, close on the basis of peak aging time to realize that grain boundaries are precipitated in opposite directions in η phase (MgZn2) Transformation and roughening, while be conducive to precipitate free zone formation, improve the stress corrosion resistant ability of alloy;4th step, timeliness Subzero treatment again afterwards can realize the precipitation again of solute since matrix belongs to supersaturated solid in deep cooling.Thermodynamics Studies have shown that in the case of deep cooling, mutually with the free energy difference very little of η phase, the driving force very little of phase transition is not susceptible to change η ', Therefore avoid strengthening the transformation of opposite stable phase while improving hardening constituent disperse educt density realizing, improve alloy strength with Toughness.
Compared with prior art, it is the advantages of technical solution of the present invention:
1. the present invention proposes to optimize the reinforcing facies type of aluminium alloy by adjusting main alloying element, guarantee alloy strength with While toughness, there is high harden ability.I.e. on the basis of Mg content, high Zn content is mentioned, realizes MgZn2In casting process It is primary to be precipitated, and reduce Cu suitably to control the S phase (Al of brittleness and difficult solid solution2) and θ phase (Al CuMg2Cu)。
2. being deep cooling after deformation, it is therefore an objective to be realized and be replied using deformation residual stress and shrinkage stress, refine the same of crystal grain When reduce matrix energy, reduce the driving force grown up of solid solution process forming core, reach grain refinement effect.
3. three-stage solution combines when low temperature is long with high temperature, short time, the η phase (MgZn for first allowing easily decomposition to be spread2) back dissolving, Solid solubility temperature is improved again, avoids realizing S phase (Al as far as possible while burning2) and θ phase (Al CuMg2Cu solid solution), it is most laggard The solid solution of the row third level improves temperature to obtain high supersaturated solid solution, provides good matrix for Precipitation.
4. subzero treatment again after timeliness can realize solute since matrix belongs to supersaturated solid in deep cooling It is precipitated again.In the case of thermodynamic study shows deep cooling, η ' is mutually with the free energy difference very little of η phase, and the driving force of phase transition is very It is small, it is not susceptible to change, therefore avoid strengthening turning for opposite stable phase while improving hardening constituent disperse educt density realizing Become, improves alloy strength and toughness.
5. compared with existing such aluminium alloy, by technical solution of the present invention without improve cost, it can be achieved that strength and toughness and The comprehensive performance of high-hardenability.
6. discharging in preparation and heat treatment process of the invention without waste water and gas, pollution-free, the requirement for equipment is lower, Be conducive to industrialized production and popularization and application.
Detailed description of the invention
The process flow chart of Fig. 1 Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy of the present invention;
Fig. 2 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 4) high-resolution-ration transmission electric-lens HRTEM figure;
Fig. 3 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample 4) by content of the present invention with the preparation of when technique Selected diffraction spot SAED figure;
Fig. 4 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 4) stretching fracture;
Fig. 5 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 15) transmission electron microscope TEM figure;
Fig. 6 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 15) the back scattering Electronic Speculum BSK figure after three-stage solution;
Fig. 7 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 15) the scanning electron microscopic picture squeezed after subzero treatment, display deep cooling are conducive to reply, and eliminate residual stress and refine crystal grain;
Fig. 8 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 18) back scattering Electronic Speculum BSK figure and power spectrum EDS;
Fig. 9 is the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample by content of the present invention with the preparation of when technique 20) the transmission electron microscope TEM figure after timeliness deep cooling;
Figure 10 is not by the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample (sample 23) of content of the present invention proportion preparation Back scattering Electronic Speculum BSK figure and power spectrum EDS.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be further described.
Example 1: by the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample of content of the present invention proportion in different heat treatment technique Under performance compare
According to each element mass percent ingredient in Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy: Zn 8.5%, Mg 2.0%, Cu 1.5%, Zr 0.12%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, Total impurities < 0.15%, surplus Al.Melting (i.e. alloying), cleaning molten and crystal grain refinement processing, cast molding form casting Ingot, demoulding are air-cooled.Cleaning molten uses N2Refining.Smelting temperature is controlled at 750-770 DEG C, is subject to and is surveyed liquidus temperature.Ingot casting Using compound Homogenization Treatments: 430 DEG C heat preservation 46 hours after be warming up to 467 DEG C of heat preservation 4h, come out of the stove air-cooled.Hot extrusion at 420 DEG C Pressure, extrusion cylinder, mold, cushion temperature be 440 DEG C.It is then handled under heat treatment process, comparison double_stage guide and three-level are solid Molten, single-stage aging and two-stage time effect, twin-stage deep cooling and three-level cryogenic technology, the concrete technology of implementation are shown in Table 1, the performance test results It is shown in Table 2.From the performance test results as it can be seen that sample 4, i.e., heat treatment process according to the present invention can allow Al-Zn-Mg-Cu system super The comprehensive performance of high strength alumin ium alloy is optimal.Attached drawing 1 is the high-resolution-ration transmission electric-lens HRTEM figure of sample 4, as the result is shown the material Expect that the Dispersed precipitate of matrix metastable phase, attached drawing 2 are corresponding selected diffraction spot SAED figures, shows the type of disperse phase, attached drawing 3 is The stretching fracture of counter sample embodies the ductile rupture of alloy.
Al-Zn0.085-Mg0.02-Cu0.015 alloy sample that 1 different heat treatment technique of table obtains (sample 4 be by It is obtained according to treatment process of the present invention)
The performance of 2 Al-Zn0.085-Mg0.02-Cu0.015 alloy sample of table compares
Example 2: by the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy sample of content of the present invention proportion in different heat treatment technique Under performance compare
According to each element mass percent ingredient in the strong aluminium aluminium alloy of Al-Zn-Mg-Cu system superelevation: Zn 9.5%, Mg 2.5%, Cu 1.9%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, Total impurities < 0.15%, surplus Al.Melting, homogenization are identical as example 1 as extrusion process, are squeezed by hot extrusion It is processed under different heat treatment process after part.Different schemes is chosen, double_stage guide and three-stage solution are compared, it is solid to compare whole grade The influence of solubility temperature compares the influence of two-stage time effect high temperature aging temp, comparison level-one deep cooling, second level deep cooling and three-level deep cooling The influence of technique.The concrete technology of implementation is shown in Table 3, and the performance test results are shown in Table 4.From the performance test results as it can be seen that sample 15, i.e., Under heat treatment process of the invention, the comprehensive performance of obtained aluminium alloy is optimal.Attached drawing 4 is the transmission electron microscope TEM of sample 15 Figure, the interrupted distribution of the Dispersed precipitate of the metastable phase of the material matrix and crystal boundary stable phase as the result is shown, attached drawing 5 is sample 15 Back scattering Electronic Speculum BSK figure after three-stage solution, display three-stage solution improve the supersaturation of matrix in the case where non-burning Degree, attached drawing 6 are that sample 15 squeezes the scanning electron microscopic picture after subzero treatment, and display deep cooling is conducive to reply, and eliminates residual stress simultaneously Refine crystal grain.
(sample 15 is for Al-Zn0.095-Mg0.025-Cu0.019 alloy sample that 3 different heat treatment technique of table obtains It is obtained according to technique of the present invention)
The performance of 4 Al-Zn0.095-Mg0.025-Cu0.019 alloy sample of table compares
Example 3: performance of the different components alloy under heat treatment process of the present invention compares
Composition design criteria according to the present invention, devise five kinds of ultra-high-strength aluminum alloys (5) sample 17-21, is shown in Table, and It is handled according to heat treatment process proposed by the invention.Meanwhile in order to compare, lists two kinds and do not carry out main conjunction by the present invention (sample 22-23 is shown in Table composition 5) and performance to the alloy of gold element design.Alloy is smelting, at cleaning molten and crystal grain refinement After reason, cast molding, demoulding is air-cooled.Smelting temperature is controlled at 750-770 DEG C, is subject to and is surveyed liquidus temperature.Ingot casting is using compound Homogenization Treatments: 430 DEG C heat preservation 46 hours after be warming up to 467 DEG C of heat preservation 4h, come out of the stove air-cooled.Hot extrusion at 420 DEG C, extrusion cylinder, Mold, cushion temperature be 440 DEG C.Subsequent subzero treatment keeps the temperature 36 hours at -197 DEG C.It is dissolved again, 470 DEG C keep the temperature 40 points It is warming up to 480 DEG C of heat preservations after clock and is warming up within 20 minutes 490 DEG C of heat preservations 20 minutes, then water quenching again.Two-stage time effect, 135 DEG C of heat preservations It is warming up to 190 DEG C after 16 hours and keeps the temperature 10 minutes.Subzero treatment keeps the temperature 36 hours at -197 DEG C.Properties of sample test result is shown in Table 6.Guarantee that yield strength is higher than 650MPa by five kinds of alloys (sample 17-21) that the present invention designs, tensile strength is higher than 650MPa, while elongation percentage is higher than 11%.The master alloying content highest of sample 20, therefore the volume fraction highest of hardening constituent are right The intensity highest answered, elongation percentage are slightly lower.The master alloying content of sample 17 is minimum, therefore the volume fraction of hardening constituent is minimum, corresponding Intensity it is minimum.Sample 18 is equally Cu content having the same relative to sample 17, therefore Zn content is with the promotion of Mg content It need to improve simultaneously, just can guarantee the comprehensive performance of alloy.Fig. 8 is the as cast condition backscattered electron photo of sample 18, can be with Zn content Promotion inhibit coarse S phase (Al2CuMg generation).Sample 20 is relative to sample 18 and sample 19, Cu having the same Content, therefore while the promotion of Mg content, it is necessary to Zn content is promoted, to guarantee η phase (MgZn2) volume fraction, to protect Demonstrate,prove alloy strength and plasticity.Fig. 9 is transmission electron microscope picture of the sample 20 after final deep cooling, can clearly see that crystal boundary is precipitated The interrupted distribution of phase.Not there is no high Cu content and low Zn content by the sample 22 that the present invention designs, cause hardening constituent S phase (Al2) and θ phase (Al CuMg2Cu component) increases, and η phase (MgZn2) volume fraction reduce, intensity and elongation percentage performance are not It is good.Sample 23 improves Zn content relative to alloy F, but still has high Cu content and low Zn content, although improving η Phase (MgZn2) volume fraction, but not inhibit S phase (Al2) and θ phase (Al CuMg2Cu component), though therefore intensity promoted, But elongation percentage is bad.Fig. 9 is the as cast condition backscattered electron photo of sample 23, it can be seen that coarse S phase (Al2CuMg)。
The aluminium alloy composition list (wt%) that table 5 is obtained according to treatment process of the present invention
The aluminium alloy capability list that table 6 is obtained according to treatment process of the present invention

Claims (9)

1. a kind of preparation method of Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy, which is characterized in that comprise the steps of:
(1) it is handled by alloy composition through ingredient, melting, cleaning molten and crystal grain refinement, cast molding forms ingot casting, demoulding sky Cold: at 750-770 DEG C, cleaning molten uses N for smelting temperature control2Refining;
(2) to step (1) ingot casting use compound Homogenization Treatments: 430 DEG C heat preservation 46 hours after be warming up to 467 DEG C of heat preservation 4h, so After come out of the stove it is air-cooled;
(3) carry out hot extrusion to the ingot casting after step (2) compound Homogenization Treatments: when extruding, metal temperature is 400~440 DEG C, Heating time is 2h;Extrusion cylinder, mold, cushion temperature be 440~480 DEG C, heating time 12h;
(4) subzero treatment is carried out to the resulting extrusion of step (3): keeps the temperature 36 hours at -197 DEG C;
(5) three-stage solution: 450~470 DEG C of heat preservations 20~heat up after forty minutes is carried out to the resulting subzero treatment sample of step (4) 20 minutes are kept the temperature to 470~480 DEG C and is warming up to 480~490 DEG C of heat preservations 20 minutes again, then water quenching or oil quenching;
(6) two-stage time effect carried out to the resulting solid solution sample of step (5): 120~135 DEG C be warming up to 180 after heat preservation 12 hours~ 190 DEG C of heat preservations are warming up to 190 DEG C for 10 minutes again and keep the temperature 20 minutes;
(7) subzero treatment is carried out to step (6) resulting aging samples again: keeping the temperature 36 hours at -197 DEG C.
2. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 7.2~9.5%, Mg 1.2~2.5%, Cu 1.3~1.9%, Zr 0.08~0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
3. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 8.5%, Mg 2.0%, Cu 1.5%, Zr 0.12%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
4. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 9.5%, Mg 2.5%, Cu 1.9%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
5. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 8.0%, Mg 2.0%, Cu 1.9%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
6. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 8.5%, Mg 2.2%, Cu 1.9%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
7. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 8.7%, Mg 2.3%, Cu 1.8%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
8. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 9.3%, Mg 2.5%, Cu 1.8%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
9. the Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy that one kind is prepared method according to claim 1, it is characterised in that: institute State aluminium alloy each component and its mass percent are as follows: Zn 9.0%, Mg 2.4%, Cu 1.8%, Zr 0.15%, Ti 0.05%, Mn 0.05%, Cr 0.04%, Fe < 0.05%, Si < 0.05%, total impurities < 0.15%, surplus Al.
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