CN103993211A - 720-750MPa super strength non-rapid-solidification aluminum alloy and preparation method thereof - Google Patents
720-750MPa super strength non-rapid-solidification aluminum alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a 720-750MPa super strength non-rapid-solidification aluminum alloy and a preparation method thereof. The alloy is characterized by mainly comprising following components by mass percent: 10.78-11.54% of zinc, 2.78-3.51% of magnesium, 2.26-2.59% of copper, 0.221-0.24% of zirconium, 0.0025-0.0465% of strontium, and the balance of aluminum and impurities. The preparation method comprises the steps of (1) casting; (2) homogenizing annealing; (3) hot extruding; (4) pre-recovery annealing; (5) solution treatment; (6) pre-plastic deformation (2%); and (7) aging treatment. The alloy has the advantages of small grain (the average grain size is about 3.26-5.563mu m), many low angle grain boundaries (the proportion of the low angle grain boundary is about 66.8-79.38%), highest strength of 759.2MPa and the elongation of 8.0%.
Description
Technical field
The present invention relates to a kind of aluminum alloy materials, especially a kind of novel 7000 line aluminium alloys and preparation method thereof, the specifically non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength.
Background technology
High strength alumin ium alloy has the features such as low density, high strength, high tenacity, corrosion-resistant, easy processing, low cost, easily recovery, environmental friendliness, is the primary structure material of aircraft.For a long time, the higher aluminium alloy of development intensity rank receives much concern always.
The mid-90 in 20th century, developed country utilizes reaction-injection moulding flash set technology successfully to develop system respectively to have gone out strong 7000 line aluminium alloys of 750MPa intensity level superelevation, and its exemplary alloy is RSA-7034(Al-11Zn-2.3Mg-1Cu), march at the forefront of the world.But aluminium alloy price prepared by reaction-injection moulding flash set technology is high, and is difficult to prepare large-scale ingot blank, has limited widespread use.
In order to ensure that 7000 line aluminium alloys have superstrength, the content of the alloy elements such as the zinc (Zn) of alloy, magnesium (Mg), copper (Cu) must be high, so that by the superstrength of separating out in a large number guarantee alloy of aging precipitation phase.Except composition, technology of preparing is also very crucial.Pre-reply moved back on the basis that processing can obviously not grow up at alloy grain, and alloy structure is replied, and reduces the recrystallize motivating force of alloy in the time of solid solution, is convenient to retain low-angle boundary after alloy solid solution, significantly improves the intensity of alloy.Predeformation can be introduced dislocation, improves alloy strength on the one hand by dislocations strengthening, and the position of separating out of a large amount of aging precipitation phases is provided on the other hand, makes separating out of aging precipitation phase more tiny, even, improves alloy strength.
Existing thermal treatment process is often difficult to take into account mechanical property and the corrosion resistance of high-alloying 7000 line aluminium alloy alloyings, tend to cause the situation of favouring one and slighting the other to occur, this will seriously restrict the use of high-alloying 7000 line aluminium alloys, so need a kind of processing method badly and effectively improve the over-all properties of high-alloying 7000 line aluminium alloys.
Up to the present, not yet have a kind of non-Solidified Al Alloy And Preparation Method of 720-750MPa superstrength with independent intellectual property right available, this has restricted the industrial expansions such as China's aerospace, weaponry to a certain extent.
Summary of the invention
The object of the invention is the large problem of shaping difficulty that mostly adopts rapid solidification to cause for strong 7000 line aluminium alloys of 750MPa intensity level superelevation, invent the non-rapid solidification aluminium alloy of a kind of 720-750MPa superstrength, its preparation method is provided simultaneously.
One of technical scheme of the present invention is:
The non-rapid solidification aluminium alloy of a kind of 720-750MPa superstrength, it is characterized in that: it is mainly made up of aluminium (Al), zinc (Zn), magnesium (Mg), copper (Cu), zirconium (Zr) and strontium (Sr), wherein, the mass percent of zinc (Zn) is 10.78 ~ 11.54%, the mass percent of magnesium (Mg) is 2.78 ~ 3.51%, the mass percent of copper (Cu) is 2.26 ~ 2.59%, the mass percent of zirconium (Zr) is 0.221 ~ 0.24%, the mass percent of strontium (Sr) is 0.0025 ~ 0.0465%, and surplus is aluminium and a small amount of impurity element.Described zinc (Zn), magnesium (Mg), its total mass degree of copper (Cu) are 16.15 ~ 17.31%.
Two of technical scheme of the present invention is:
A preparation method for the non-rapid solidification aluminium alloy of 720-750MPaa superstrength, is characterized in that it comprises successively: (1) founding; (2) homogenizing anneal; (3) hot extrusion; (4) pre-recovery annealing; (5) solution treatment; (6) predeformation and (7) ageing treatment;
Described founding refers to and will after pure Al fusing, add successively Al-Cu master alloy, Al-Sr master alloy, Al-Zr master alloy, pure Zn and pure Mg, after all master alloy fusings, add again hexachloroethane refining degasification until do not have gas to overflow, after leaving standstill insulation 5 ~ 10 min, remove slag and be cast into ingot, in described Al-Cu master alloy, the mass percent of Cu is 50.12%, in Al-Sr master alloy, the mass percent of Sr is that the mass percent of Zr in 9.89%, Al-Zr master alloy is 4.11%;
Described homogenizing anneal refers to the alloy of founding gained is respectively to 400 ± 5 DEG C × 6h through excess temperature successively, 420 ± 5 DEG C × 6h, anneals for four times of 440 ± 5 DEG C × 6h and 460 ± 5 DEG C × 12h;
Described hot extrusion refer to by be heated to through the alloy of homogenizing anneal 480 ± 5 DEG C and be incubated 8h after to carry out extrusion ratio be 12 hot extrusion;
Described pre-recovery annealing refers to anneals the alloy through hot extrusion again through four times of 250 ± 5 DEG C × 24 h, 300 ± 5 DEG C × 6 h, 350 ± 5 DEG C × 6 h and 400 ± 5 DEG C × 6 h;
Described solution treatment refers to and will carry out 450 ± 5 DEG C × 2h, 460 ± 5 DEG C × 2h through the alloy of pre-recovery annealing and 470 ± 5 DEG C × 2h is incubated processing, then at room temperature carries out shrend;
Described predeformation is to instigate through the alloy of solution treatment to carry out 2% viscous deformation;
Described ageing treatment refers to carries out the alloy through predeformation 121 ± 5 DEG C × 24h or carries out the ageing treatment that 121 ± 5 DEG C × 5h adds 133 ± 5 DEG C × 16h.
Above-mentioned each preparation technology's optimum temps is respectively:
Four annealing temperatures of homogenizing anneal are respectively 400 DEG C, and 420 DEG C, 440 DEG C and 460 DEG C; Extrusion temperature is 480 DEG C; Pre-annealing temperature is respectively 250 DEG C, 300 DEG C, 350 DEG C and 400 DEG C; Solid solution temperature is respectively 450 DEG C, 460 DEG C and 470 DEG C; Aging temperature is respectively 121 DEG C or 121 DEG C and adds 133 DEG C.
Beneficial effect of the present invention:
(1) the present invention has obtained composition of the non-rapid solidification aluminium alloy of a kind of 720-750MPa superstrength and preparation method thereof.
(2) alloy grain of the present invention tiny (its average grain size is about 3.26 ~ 5.563 μ m), low angle grain boundary many (its low angle grain boundary ratio is about 66.8 ~ 79.38%), maximum intensity can reach 759.2MPa simultaneously unit elongation be 8.0%.
Brief description of the drawings
Fig. 1 is that the EBSD of the embodiment of the present invention one organizes photo.
Fig. 2 is the grain size distribution figure of the embodiment of the present invention one.
Fig. 3 is the crystal boundary angular distribution figure of the embodiment of the present invention one.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Embodiment mono-
As shown in Figure 1, 2, 3.
The non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength:
Be formulated as example by 28kg aluminium alloy.
First by the pure Al(composition of 20.55 kg A00 grade: 99.79%Al, 0.14%Fe, 0.04%Si, the all components of the present invention all adopt mass percent to represent, lower same, the part that all components is added less than 100% is impurity) add successively 1.54 kgAl-Cu (49.62%Al after fusing, 50.12%Cu, 0.15%Fe, 0.11%Si) master alloy (rate of loss of Cu is about 6.25%), 0.53 kg Al-Sr (89.86%Al, 9.89%Sr, 0.15%Fe, 0.10%Si) master alloy (rate of loss of Sr is about 75%), 1.64 kg Al-Zr master alloy (95.69%Al, 4.11%Zr, 0.20%Fe, 0.10%Si) (rate of loss of Zr is about 8%), the pure Zn of 3.28 kg (rate of loss of Zn is about 8%), the pure Mg of 0.97 kg (rate of loss of Mg is about 20%), described master alloy can directly be purchased from the market, also can adopt ordinary method to prepare voluntarily, after the medium front a kind of master alloy of melting process or melting of metal, add rear a kind of master alloy or metal, (add-on is 56 g) until there is no gas overflowing after being all melted to successively in aluminum solutions, to add hexachloroethane refining, leave standstill insulation 5 ~ 10 min and remove slag after be cast into ingot, become the alloy of ingot to carry out successively carrying out after 400 DEG C × 6h+420 DEG C × 6h+440 DEG C × 6h+460 DEG C × homogenizing anneal of 12h, 480 DEG C of insulation 8h room temperature shrend solution treatment after pre-recovery annealing that extrusion ratio is 12 extruding, 250 DEG C × 24 h+300 DEG C × 6 h+350 DEG C × 6 h+400 DEG C × 6 h, 450 DEG C × 2h+460 DEG C × 2h+470 DEG C × 2h insulation, the predeformation of 2% viscous deformation, the ageing treatment of 121 DEG C × 24h to founding, obtain the non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength.
The aluminium alloy of the present embodiment through spectrum actual measurement composition is: 10.78%Zn, and 2.78%Mg, 2.59%Cu, 0.221%Zr, 0.0465%Sr, surplus is aluminium and impurity element.
The aluminium alloy grain-size of the present embodiment is tiny, and its average grain size is 5.563 μ m(accompanying drawings 1, accompanying drawing 2), low angle grain boundary quantity is many, its low angle grain boundary ratio is 66.8%(accompanying drawing 3), observed strength is that 728 MPa, unit elongation are 7.0%.
Embodiment bis-
The non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength:
Be formulated as example by 28kg aluminium alloy.
First by the pure Al(composition of 20.68 kg A00 grade: 99.79%Al, 0.14%Fe, 0.04%Si, the all components of the present invention all adopt mass percent to represent, lower same, the part that all components is added less than 100% is impurity) add successively 1.35 kgAl-Cu (49.62%Al after fusing, 50.12%Cu, 0.15%Fe, 0.11%Si) master alloy (rate of loss of Cu is about 6.25%), 0.028 kg Al-Sr (89.86%Al, 9.89%Sr, 0.15%Fe, 0.10%Si) master alloy (rate of loss of Sr is about 75%), 1.78 kg Al-Zr master alloy (95.69%Al, 4.11%Zr, 0.20%Fe, 0.10%Si) (rate of loss of Zr is about 8%), the pure Zn of 3.51 kg (rate of loss of Zn is about 8%), the pure Mg of 1.20 kg (rate of loss of Mg is about 20%), described master alloy can directly be purchased from the market, also can adopt ordinary method to prepare voluntarily, after the medium front a kind of master alloy of melting process or melting of metal, add rear a kind of master alloy or metal, (add-on is 56 g) until there is no gas overflowing after being all melted to successively in aluminum solutions, to add hexachloroethane refining, leave standstill insulation 5 ~ 10 min and remove slag after be cast into ingot, become the alloy of ingot to carry out carrying out after 400 DEG C × 6h+420 DEG C × 6h+440 DEG C × 6h+460 DEG C × homogenizing anneal of 12h, 480 DEG C of insulation 8h room temperature shrend solution treatment after pre-recovery annealing that extrusion ratio is 12 extruding, 250 DEG C × 24 h+300 DEG C × 6 h+350 DEG C × 6 h+400 DEG C × 6 h, 450 DEG C × 2h+460 DEG C × 2h+470 DEG C × 2h insulation, the predeformation of 2% viscous deformation, the ageing treatment of 121 DEG C × 24h to founding, obtain the non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength.
The aluminium alloy of the present embodiment through spectrum actual measurement composition is: 11.54%Zn, and 3.51%Mg, 2.26%Cu, 0.24Zr%, 0.0025%Sr, surplus is aluminium and impurity element.
The aluminium alloy of the present embodiment
The aluminium alloy grain-size of the present embodiment is tiny, and its average grain size is 3.26 μ m, and low angle grain boundary quantity is many, and its low angle grain boundary ratio is 66.8%, and observed strength is that 727.7MPa, unit elongation are 6.4%.
Embodiment tri-.
The non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength:
Be formulated as example by 28kg aluminium alloy.
First by the pure Al(composition of 20.65 kg A00 grade: 99.79%Al, 0.14%Fe, 0.04%Si, the all components of the present invention all adopt mass percent to represent, lower same, the part that all components is added less than 100% is impurity) add successively 1.45 kgAl-Cu (49.62%Al after fusing, 50.12%Cu, 0.15%Fe, 0.11%Si) master alloy (rate of loss of Cu is about 6.25%), 0.040 kg Al-Sr (89.86%Al, 9.89%Sr, 0.15%Fe, 0.10%Si) master alloy (rate of loss of Sr is about 75%), 1.68 kg Al-Zr master alloy (95.69%Al, 4.11%Zr, 0.20%Fe, 0.10%Si) (rate of loss of Zr is about 8%), the pure Zn of 3.50 kg (rate of loss of Zn is about 8%), the pure Mg of 1.23 kg (rate of loss of Mg is about 20%), described master alloy can directly be purchased from the market, also can adopt ordinary method to prepare voluntarily, after the medium front a kind of master alloy of melting process or melting of metal, add rear a kind of master alloy or metal, (add-on is 56 g) until there is no gas overflowing after being all melted to successively in aluminum solutions, to add hexachloroethane refining, leave standstill insulation 5 ~ 10 min and remove slag after be cast into ingot, become the alloy of ingot to carry out carrying out after 400 DEG C × 6h+420 DEG C × 6h+440 DEG C × 6h+460 DEG C × homogenizing anneal of 12h, 480 DEG C of insulation 8h room temperature shrend solution treatment after pre-recovery annealing that extrusion ratio is 12 extruding, 250 DEG C × 24 h+300 DEG C × 6 h+350 DEG C × 6 h+400 DEG C × 6 h, 450 DEG C × 2h+460 DEG C × 2h+470 DEG C × 2h insulation, the predeformation of 2% viscous deformation, the ageing treatment of 121 DEG C × 24h to founding, obtain the non-Solidified Al Alloy And Preparation Method of a kind of 720-750MPa superstrength.
Embodiment tetra-
Roughly the same, difference is that aging treatment process changes 121 DEG C × 5h+133 DEG C × 16h into for the present embodiment and embodiment mono-.
The observed strength of the aluminium alloy of the present embodiment is that 754.45 MPa, unit elongation are 7.0%.
Embodiment five
Roughly the same, difference is that aging treatment process changes 121 DEG C × 5h+133 DEG C × 16h into for the present embodiment and embodiment bis-.
The observed strength of the aluminium alloy of the present embodiment is that 759.2MPa, unit elongation are 8.0%.
Embodiment six
The difference of the present embodiment and embodiment mono-to five is that each technological temperature rises or declines 5 DEG C, and all the other processing condition are constant.The end properties of gained and embodiment mono-to five are roughly the same, and error is less than 1%.
Below only listed proportioning and the manufacture method of the aluminium alloy of several common proportionings, those skilled in the art can suitably adjust the proportioning of each component and strictly can obtain the non-Solidified Al Alloy And Preparation Method of desirable 720-750MPa superstrength by above-mentioned steps manufacture according to above-mentioned example.
The part that the present invention does not relate to all prior art that maybe can adopt same as the prior art is realized.
Claims (4)
1. the non-rapid solidification aluminium alloy of 720-750MPa superstrength, it is characterized in that: it is mainly made up of aluminium (Al), zinc (Zn), magnesium (Mg), copper (Cu), zirconium (Zr) and strontium (Sr), wherein, the mass percent of zinc (Zn) is 10.78 ~ 11.54%, the mass percent of magnesium (Mg) is 2.78 ~ 3.51%, the mass percent of copper (Cu) is 2.26 ~ 2.59%, the mass percent of zirconium (Zr) is 0.221 ~ 0.24%, the mass percent of strontium (Sr) is 0.0025 ~ 0.0465%, and surplus is aluminium and a small amount of impurity element.
2. aluminium alloy according to claim 1, is characterized in that the mass percentage content of described zinc (Zn), magnesium (Mg) and copper (Cu) three sum is 16.15 ~ 17.31%.
3. a preparation method for the non-rapid solidification aluminium alloy of 720-750MPaa superstrength claimed in claim 1, is characterized in that it comprises successively: (1) founding; (2) homogenizing anneal; (3) hot extrusion; (4) pre-recovery annealing; (5) solution treatment; (6); Predeformation and (7) ageing treatment;
Described founding refers to and will after pure Al fusing, add successively Al-Cu master alloy, Al-Sr master alloy, Al-Zr master alloy, pure Zn and pure Mg, after all master alloy fusings, add again hexachloroethane refining degasification until do not have gas to overflow, after leaving standstill insulation 5 ~ 10 min, remove slag and be cast into ingot, in described Al-Cu master alloy, the mass percent of Cu is 50.12%, in Al-Sr master alloy, the mass percent of Sr is that the mass percent of Zr in 9.89%, Al-Zr master alloy is 4.11%;
Described homogenizing anneal refers to the alloy of founding gained is respectively to 400 ± 5 DEG C × 6h through excess temperature successively, 420 ± 5 DEG C × 6h, anneals for four times of 440 ± 5 DEG C × 6h and 460 ± 5 DEG C × 12h;
Described hot extrusion refer to by be heated to through the alloy of homogenizing anneal 480 ± 5 DEG C and be incubated 8h after to carry out extrusion ratio be 12 hot extrusion;
Described pre-recovery annealing refers to anneals the alloy through hot extrusion again through four times of 250 ± 5 DEG C × 24 h, 300 ± 5 DEG C × 6 h, 350 ± 5 DEG C × 6 h and 400 ± 5 DEG C × 6 h;
Described solution treatment refers to and will carry out 450 ± 5 DEG C × 2h, 460 ± 5 DEG C × 2h through the alloy of pre-recovery annealing and 470 ± 5 DEG C × 2h is incubated processing, then at room temperature carries out shrend;
Described predeformation is to instigate through the alloy of solution treatment to carry out 2% viscous deformation;
Described ageing treatment refers to carries out the alloy through predeformation 121 ± 5 DEG C × 24h or carries out the ageing treatment that 121 ± 5 DEG C × 5h adds 133 ± 5 DEG C × 16h.
4. method according to claim 3, is characterized in that four annealing temperatures of described homogenizing anneal are respectively 400 DEG C, 420 DEG C, and 440 DEG C and 460 DEG C; Described extrusion temperature is 480 DEG C; Described pre-annealing temperature is respectively 250 DEG C, 300 DEG C, 350 DEG C and 400 DEG C; Described solid solution temperature is respectively 450 DEG C, 460 DEG C and 470 DEG C; Described aging temperature is respectively 121 DEG C or 121 DEG C and adds 133 DEG C.
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| CN106367701A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | Method for improving performance of ultrahigh-strength aluminum alloy |
| CN107460382A (en) * | 2017-08-18 | 2017-12-12 | 江苏大学 | The superpower Alcoa rolled plate of isotropism and preparation method |
| CN109457154A (en) * | 2019-01-07 | 2019-03-12 | 江苏豪然喷射成形合金有限公司 | A kind of heat treatment process of 7055 aluminium alloy |
| CN111101032A (en) * | 2019-12-18 | 2020-05-05 | 山东南山铝业股份有限公司 | High-strength and high-plasticity extruded aluminum alloy and preparation method thereof |
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| CN111101032A (en) * | 2019-12-18 | 2020-05-05 | 山东南山铝业股份有限公司 | High-strength and high-plasticity extruded aluminum alloy and preparation method thereof |
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