CN113373354A - Ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and preparation process thereof - Google Patents
Ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and preparation process thereof Download PDFInfo
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- 238000005096 rolling process Methods 0.000 claims abstract description 46
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 44
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims description 57
- 238000005266 casting Methods 0.000 claims description 27
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- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 238000003723 Smelting Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000005098 hot rolling Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000005728 strengthening Methods 0.000 claims description 6
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- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
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- C22C21/10—Alloys based on aluminium with zinc as the next major constituent
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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Abstract
The invention relates to an ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and a preparation process thereof, wherein the alloy components comprise Zn6.5-7%, Mg 1.8-2.3%, Cu 1.9-2.4%, Sc 0.18-0.22%, Zr 0.08-0.12%, Si less than or equal to 0.1%, Fe less than or equal to 0.15%, Mn less than or equal to 0.05%, Cr less than or equal to 0.04%, Ti less than or equal to 0.06% and the balance of Al. During preparation, after melting, pouring and heat preservation are carried out according to the proportion, an alloy plate is obtained by rolling, and the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate is prepared by (480-160 ℃) x (0.5-1.5h) solution treatment and (140-160 ℃) x (17-19h) + (190-210 ℃) x (0.5-1.5h) + (150-170 ℃) regression re-aging treatment.
Description
The technical field is as follows:
the invention belongs to the technical field of alloy plate preparation, and particularly relates to an ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and a preparation process thereof.
Background art:
the 7XXX series alloys were developed on the basis of Al-Zn-Mg alloys by adding Cu, which has a strength higher than that of the 2XXX series alloys, commonly referred to as ultra-high strength aluminum alloys. The ultrahigh-strength aluminum alloy has the advantages of low density, high specific strength, good hot workability and the like, and the research and the application of the ultrahigh-strength aluminum alloy are concerned all the time.
The first 7XXX series alloys were proposed by weber in 1932, and the first high strength Al-Zn-Mg-Cu based alloys in the world were developed by adding Cu along with a small amount of Mn. But has not been put to practical use because of the high stress corrosion Sensitivity (SCC) of the alloy. In 1936, Isglan, a Japanese scholars, added Cr to Al-Zn-Mg-Cu alloy for the first time, developed a famous ESD super-hard alloy (Al-7.5% Zn-l.5% Mg-2% Cu-0.6% Mn-0.25% Cr), which has strength of over 600MPa and better stress corrosion resistance, and the alloy is firstly put into practical use in the aircraft manufacturing industry. On the basis of the research of ESD alloy, a batch of 7xxx series aluminum alloy containing small amount of Cr and Mn is developed in each country. The 7075 alloy was developed in the United states of 1943 and is applied to a B-29 bomber for the first time, which brings revolutionary changes to the structure and performance of the airplane and lays a foundation for the rapid development of ultra-high strength aluminum alloy. In 1954, 7178-T651 alloy with higher strength than 7075-T651 alloy was developed by increasing the contents of Zn, Mg and Cu on the basis of 7075 alloy. This alloy, although high in strength, was too poor in fracture toughness and was replaced by 7075-T651 alloy on Boeing 747 aircraft. In 1960, a secondary aging process T73 was developed and applied to 7075 alloy, and the problem of thick cross section SCC was solved. T76 aging was developed in the middle of the 60 sThe process improves the alloy strength compared with T73, and the stress corrosion resistance and the denudation resistance meet the use requirements. In 1968, on the basis of 7001 alloy, aluminum companies in the United states increased Mg and Zn contents and reduced Cu and Cr contents, and developed 7049 alloy. In 1969, based on 7075 alloy, 7475 alloy with the highest 7xxx fracture toughness was developed by reducing the contents of Fe and Si, controlling the content of Cr, and adjusting the contents of Mn and Cu to improve the fracture toughness, wherein the alloy has the processing technique changed except for the component difference, and the grain size, uniformity and E phase (Al) are adjusted12Mg2Cr) to improve toughness. In 1971, 7075 was used as the basis in the united states, increasing Zn, Cu content and Cu/Mg ratio to improve strength, Zr was used instead of Cr to overcome quench sensitivity problems and to adjust grain size, and 7050 alloys with higher strength, fracture toughness and stress corrosion resistance were developed and registered in the aluminum association of the united states in the same year. In the 80 s, Alcoa corporation carried out a lot of research, further reduced the content of Si and Mn impurity elements and improved the Zn/Mg ratio on the basis of 7050 and 7150 alloys, developed 7055 alloy successfully, and applied for patent in 1993. A series of high-level Al-Zn-Mg-Cu series ultrahigh-strength aluminum alloys are developed between the end of the 50 s and the end of the 80 s. In Russian aluminum alloy brands, the U-shaped nut is a Zr-containing alloy, the U-shaped nut is a high-purity alloy, and the 0 nut is the highest-purity alloy. The B95 alloy was developed in 1948, similar to the us 7075 alloy. In 1956, on the basis of intensive research on Al-Zn-Mg-Cu, Zr is added into Al-Zn-Mg-Cu alloy for the first time in the world to replace Cr, and B96 alloy with the highest alloying degree and strength is developed; b96 was developed in 1968 by reducing the content of Fe impurity and adding Mn elementЦ-1Alloying; in 1970, B96 with better plasticity and slightly reduced strength was developed by further reducing the content of Fe and Si impurities and reducing the content of main alloy elementsЦ-3. After the research of B95 alloy in 1948, the research institute of Total Su light alloy and Total Su aviation materials developed B95 in 1971 by reducing the content of Fe and Si impuritiesЦЧAnd B95OЧThese two alloys are used not only to make aircraft of the type il 96-300 and 204, but nowadays also of the type su-27 and su-30A structural member.
The research and development of the ultra-high strength aluminum alloy in China are relatively late. In the early 80 s of the 20 th century, Al-Zn-Mg-Cu aluminum alloys were developed in the northeast light alloy processing plant and the Beijing aviation material research institute. At present, China enters into the practical application stage in the production and application aspects of common 7XXX series aluminum alloy, mainly comprises 7075, 7050, 7175 and the like, and is used for manufacturing certain structural parts of aerospace craft. In the middle of the 90 s, 7A55 ultrahigh-strength aluminum alloy was successfully prepared by the Beijing aviation material research institute by a continuous casting method, and in recent years, 7A60 aluminum alloy with higher strength was developed. The research and development of ultrahigh-strength aluminum alloy with higher Zn content by adopting a spray forming process are carried out by Beijing nonferrous metal research institute and the northeast light alloy processing factory. The units such as the Beijing nonferrous metals research institute, the northeast university, the China university, the Beijing aerospace university, the Beijing technology university and the northeast light alloy processing factory jointly research the novel ultrahigh-strength high-strength alloy. The nominal composition of the alloy is A1-10% Zn-2.5% Mg-2.3% Cu-0.15% Zr. A Peking nonferrous metals research institute adopts a spray forming technology to prepare an ingot, the ingot has no cracks and small tissue, and the strength reaches 810MPa after deformation and heat treatment[19-20]. In summary, the research on the ultra-high strength aluminum alloy is developed along the directions of high strength, low toughness-high strength, high toughness and corrosion resistance; the research direction of the heat treatment state develops along T6-T73-T76-T736(T74) -T77; the development characteristics of the alloy design direction are that the alloying degree is higher and higher, the impurity content of Fe, Si and the like is lower and lower, the addition of trace transition group elements is more and more reasonable, and the final result is that the alloy is kept to have excellent toughness and corrosion resistance while the strength is greatly improved.
At present, the consumption of aluminum alloy on civil aircrafts in various countries accounts for 70-80% of the weight of the structure, wherein most of the aluminum alloy is ultrahigh-strength aluminum alloy. Therefore, the material workers in various countries have been dedicated to research and develop the ultrahigh-strength aluminum alloy integrating high strength, high toughness and high corrosion resistance for many years. The invention optimizes the component design of the 7xxx series aluminum alloy, adds the rare earth elements Sc and Zr, designs novel Al-Zn-Mg-Cu-Sc-Zr alloy components, and provides the rolling and heat treatment methods of the alloy plate.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provides an ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and a preparation process thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following components in percentage by mass: 6.5 to 7 percent of Zn, 1.8 to 2.3 percent of Mg, 1.9 to 2.4 percent of Cu, 0.18 to 0.22 percent of Sc, 0.08 to 0.12 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
The Zn is added in the form of pure Zn, the Mg is added in the form of pure Mg, the Cu is added in the form of pure Cu, the Sc is added in the form of Al-2% Sc master alloy, and the Zr is added in the form of Al-5% Zr master alloy.
The tensile strength of the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate is 705MPa to 725MPa, the yield strength is 608MPa to 632MPa, and the elongation at break is 9.2 percent to 11.5 percent.
The crystal grains of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are equiaxial, the size of the crystal grains is 60-80 mu m, and precipitated phases capable of strengthening the alloy exist in the crystal grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm.
The preparation process of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following steps:
(1) smelting and pouring the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components to obtain an alloy casting blank;
(2) carrying out heat preservation on the alloy casting blank at the temperature of 490-510 ℃ for 1-3h, and then carrying out hot rolling, wherein the initial rolling temperature is 480-490 ℃, and the final rolling temperature is 440-450 ℃ to obtain an alloy plate; wherein the rolling pass is 5-6 passes, the total reduction is 73.33-80%, and the single-pass reduction is 20-30%;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression re-aging treatment to prepare the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, and the solution treatment process parameters are (480-:
(140-160℃)×(17-19h)+(190-210℃)×(0.5-1.5h)+(150-170℃)×(17-19h)。
in the step (1), the alloy smelting temperature is 730-740 ℃; the charging sequence is as follows: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; the melt was stirred while pure Mg was added.
In the step (1), after all furnace burden is added, the scum on the surface of the melt is removed, and then sampling analysis is carried out to ensure that the components are qualified.
In the step (1), the pouring temperature is 720-730 ℃, and the filtration and deslagging in the aluminum liquid transferring process are carried out by using glass fiber cloth and a ceramic filter, wherein the filter consists of 2 layers of glass meshes and a PPI40 foamed ceramic filter core.
In the step (1), the alloy casting blank has the thickness of 30mm, the width of 200mm and the length of 500 mm.
In the step (2), the rolling speed is 0.5-2.5 m/s.
In the step (2), the bloom temperature is preferably 490 ℃.
In the step (2), the 1 st pass reduction is preferably 30%, and when the rolling pass is 5 passes, the single-pass reduction magnitude value sequence is that the 1 st pass is more than or equal to the 2 nd pass, more than or equal to the 3 rd pass, more than or equal to the 4 th pass, more than or equal to the 5 th pass; when the rolling pass is 6 passes, the single-pass reduction magnitude sequence is that the 1 st pass is more than or equal to the 2 nd pass, more than or equal to the 3 rd pass, more than or equal to the 4 th pass, more than or equal to the 5 th pass, more than or equal to the 6 th pass, namely, most of the reduction tasks are ensured to be completed in the former pass, and the reduction in the backward single-pass is gradually reduced.
In the step (2), the thickness of the alloy plate is 6-8 mm.
The invention has the beneficial effects that:
according to the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate and the preparation process thereof, a proper amount of Sc and Zr elements are added on the basis of Al-Zn-Mg-Cu alloy, a specific high-temperature regression process is added in the middle of two-stage aging through hot rolling and heat treatment, large-size precipitated phases can be redissolved, the precipitated phases are dispersed to be fine as a whole, and the alloy plate with high strength and high plasticity is obtained by controlling the alloy structure.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of a tensile fracture of Al-Zn-Mg-Cu-Sc-Zr alloy sheets prepared according to comparative examples 3 to 6 of the present invention;
FIG. 2 is a scanning electron microscope image of a tensile fracture of an Al-Zn-Mg-Cu-Sc-Zr alloy sheet prepared in example 3 of the present invention;
FIG. 3 is a scanning electron microscope image of a tensile fracture of the Al-Zn-Mg-Cu-Sc-Zr alloy sheet prepared in comparative examples 3 to 7 according to the present invention;
FIG. 4 is a graph showing the cracking of Al-Zn-Mg-Cu-Sc-Zr alloy sheets according to comparative examples 3 to 8 of the present invention;
FIG. 5 is a graph showing the cracking of Al-Zn-Mg-Cu-Sc-Zr alloy sheets prepared in comparative examples 3 to 9 according to the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
Grain sizes of ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy sheets prepared in examples 1 to 4 below, and Al3The (Sc, Zr) phase particle size is limited to the detection means and is not further divided, but actually different from each other, and the average grain size is different from that of Al3Average particle size of (Sc, Zr) phase: example 1 > example 4 > example 2 > example 3.
Example 1
The ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following components in percentage by mass: 6.5 percent of Zn, 1.8 percent of Mg, 1.9 percent of Cu, 0.18 percent of Sc, 0.08 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
The Zn is added in the form of pure Zn, the Mg is added in the form of pure Mg, the Cu is added in the form of pure Cu, the Sc is added in the form of Al-2% Sc master alloy, and the Zr is added in the form of Al-5% Zr master alloy.
The preparation process of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following steps:
(1) after smelting according to the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components, pouring to obtain an alloy casting blank, wherein the thickness of the alloy casting blank is 30mm, the width of the alloy casting blank is 200mm, and the length of the alloy casting blank is 500mm, and the method comprises the following steps:
the alloy smelting temperature is 730 ℃; the charging sequence is as follows: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; stirring the melt while adding pure Mg;
the casting temperature is 720 ℃, and the filtration and deslagging of the molten aluminum transfer process are carried out by using glass fiber cloth and a ceramic filter, wherein the filter consists of 2 layers of glass meshes and a PPI40 foamed ceramic filter core;
after all furnace burden is added, skimming dross on the surface of the melt, and then sampling and analyzing to ensure that the components are qualified;
(2) carrying out heat preservation on the alloy casting blank at 490 ℃ for 3h, and then carrying out hot rolling, wherein the initial rolling temperature is 480 ℃, the final rolling temperature is 440 ℃, the rolling pass is 5 passes, the total rolling reduction is 73.33%, the 1 st pass reduction is 30%, the 2 nd pass reduction is 22%, the 3 rd pass reduction is 21.98%, the 4 th pass reduction is 21.75%, the 5 th pass reduction is 20%, and the rolling speed is 0.5m/s, so as to obtain an alloy plate with the thickness of 8 mm;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression and reaging treatment, the technological parameters of the solution treatment are 480 ℃ multiplied by 1.5h, and the technological parameters of the regression and reaging treatment are as follows: 19h at 140 ℃, 1.5h at 190 ℃, 19h at 150 ℃; the method comprises the steps of preparing the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, wherein the crystal grains of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are equiaxial, the size of the crystal grains is 60-80 mu m, and precipitated phases capable of strengthening the alloy exist in the crystal grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm. The tensile strength is 705MPa, the yield strength is 608MPa, and the elongation at break is 10.3%.
Example 2
The ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following components in percentage by mass: 6.6 percent of Zn, 2.0 percent of Mg, 2.0 percent of Cu, 0.19 percent of Sc, 0.09 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
The Zn is added in the form of pure Zn, the Mg is added in the form of pure Mg, the Cu is added in the form of pure Cu, the Sc is added in the form of Al-2% Sc master alloy, and the Zr is added in the form of Al-5% Zr master alloy.
The preparation process of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following steps:
(1) after smelting according to the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components, pouring to obtain an alloy casting blank, wherein the thickness of the alloy casting blank is 30mm, the width of the alloy casting blank is 200mm, and the length of the alloy casting blank is 500mm, and the method comprises the following steps:
the alloy smelting temperature is 730 ℃; the charging sequence is as follows: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; stirring the melt while adding pure Mg;
the casting temperature is 720 ℃, and the filtration and deslagging of the molten aluminum transfer process are carried out by using glass fiber cloth and a ceramic filter, wherein the filter consists of 2 layers of glass meshes and a PPI40 foamed ceramic filter core;
after all furnace burden is added, skimming dross on the surface of the melt, and then sampling and analyzing to ensure that the components are qualified;
(2) carrying out heat preservation on the alloy casting blank at 490 ℃ for 3h, and then carrying out hot rolling, wherein the initial rolling temperature is 485 ℃, the final rolling temperature is 445 ℃, the rolling pass is 5 passes, the total reduction is 75%, the 1 st pass reduction is 30%, the 2 nd pass reduction is 21.9%, the 3 rd pass reduction is 20.73%, the 4 th pass reduction is 20%, the 5 th pass reduction is 27.88%, and the rolling speed is 1.5m/s, so as to obtain an alloy plate with the thickness of 7.5 mm;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression and reaging treatment, the technological parameters of the solution treatment are 485 ℃ multiplied by 1h, and the technological parameters of the regression and reaging treatment are as follows: 150 ℃ multiplied by 18h +200 ℃ multiplied by 1h +160 ℃ multiplied by 18 h; system for makingObtaining the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, wherein the crystal grains of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are equiaxial, the size of the crystal grains is 60-80 mu m, and precipitated phases capable of strengthening the alloy exist in the crystal grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm. The tensile strength is 718MPa, the yield strength is 626MPa, and the elongation at break is 10.6%.
Example 3
The ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following components in percentage by mass: 6.8 percent of Zn, 2.2 percent of Mg, 2.2 percent of Cu, 0.20 percent of Sc, 0.10 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
The Zn is added in the form of pure Zn, the Mg is added in the form of pure Mg, the Cu is added in the form of pure Cu, the Sc is added in the form of Al-2% Sc master alloy, and the Zr is added in the form of Al-5% Zr master alloy.
The preparation process of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following steps:
(1) after smelting according to the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components, pouring to obtain an alloy casting blank, wherein the thickness of the alloy casting blank is 30mm, the width of the alloy casting blank is 200mm, and the length of the alloy casting blank is 500mm, and the method comprises the following steps:
the alloy smelting temperature is 730-740 ℃; the charging sequence is as follows: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; stirring the melt while adding pure Mg;
the pouring temperature is 720-730 ℃, and the filtration and deslagging of the aluminum liquid transferring process are carried out by using glass fiber cloth and a ceramic filter, wherein the filter consists of 2 layers of glass meshes and a PPI40 foamed ceramic filter core;
after all furnace burden is added, skimming dross on the surface of the melt, and then sampling and analyzing to ensure that the components are qualified;
(2) carrying out heat preservation on the alloy casting blank at 500 ℃ for 2h, and then carrying out hot rolling, wherein the initial rolling temperature is 490 ℃, the final rolling temperature is 450 ℃, the rolling pass is 6 passes, the total rolling reduction is 80%, the 1 st pass reduction is 30%, the 2 nd pass reduction is 25%, the 3 rd pass reduction is 23%, the 4 th pass reduction is 22%, the 5 th pass reduction is 21%, the 6 th pass reduction is 20%, and the rolling speed is 1.5m/s, so that an alloy plate is obtained, and the thickness is 6 mm;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression and reaging treatment, the technological parameters of the solution treatment are 485 ℃ multiplied by 1h, and the technological parameters of the regression and reaging treatment are as follows: 150 ℃ multiplied by 18h +200 ℃ multiplied by 1h +160 ℃ multiplied by 18 h; and (3) preparing the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, wherein a scanning electron microscope image of a tensile fracture of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate is shown in figure 2. The grain size of the alloy sheet is 60-80 mu m, and precipitated phases capable of strengthening the alloy exist in the grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm. The crystal grains were equiaxed, and elongation in the rolling direction was not observed. It can be seen that, when rolling is performed and the rolling reduction satisfies a certain critical condition, sufficient dynamic recrystallization occurs, and the original coarse as-cast structure is refined. According to Hall-Petch principle, the grain refinement can realize good matching of strength and plasticity, so that the plasticity is not obviously reduced while the alloy strength is greatly improved when the total pressure is 80%. The tensile strength is 725MPa, the yield strength is 632MPa, and the elongation at break is 9.2%.
Example 4
The ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following components in percentage by mass: 7 percent of Zn, 2.3 percent of Mg, 2.4 percent of Cu, 0.22 percent of Sc, 0.12 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
The Zn is added in the form of pure Zn, the Mg is added in the form of pure Mg, the Cu is added in the form of pure Cu, the Sc is added in the form of Al-2% Sc master alloy, and the Zr is added in the form of Al-5% Zr master alloy.
The preparation process of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate comprises the following steps:
(1) after smelting according to the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components, pouring to obtain an alloy casting blank, wherein the thickness of the alloy casting blank is 30mm, the width of the alloy casting blank is 200mm, and the length of the alloy casting blank is 500mm, and the method comprises the following steps:
the alloy smelting temperature is 730-740 ℃; the charging sequence is as follows: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; stirring the melt while adding pure Mg;
the pouring temperature is 720-730 ℃, and the filtration and deslagging of the aluminum liquid transferring process are carried out by using glass fiber cloth and a ceramic filter, wherein the filter consists of 2 layers of glass meshes and a PPI40 foamed ceramic filter core;
after all furnace burden is added, skimming dross on the surface of the melt, and then sampling and analyzing to ensure that the components are qualified;
(2) carrying out heat preservation on the alloy casting blank at 510 ℃ for 1h, and then carrying out hot rolling, wherein the initial rolling temperature is 490 ℃, the final rolling temperature is 450 ℃, the rolling pass is 5 passes, the total reduction is 75%, the 1 st pass reduction is 30%, the 2 nd pass reduction is 21.9%, the 3 rd pass reduction is 20.73%, the 4 th pass reduction is 20%, the 5 th pass reduction is 27.88%, and the rolling speed is 2.5m/s, so as to obtain an alloy plate with the thickness of 7.5 mm;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression and reaging treatment, the technological parameters of the solution treatment are 490 ℃ multiplied by 0.5h, and the technological parameters of the regression and reaging treatment are as follows: 160 ℃ multiplied by 17h +210 ℃ multiplied by 0.5h +170 ℃ multiplied by 17 h; the method comprises the steps of preparing the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, wherein the crystal grains of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are equiaxial, the size of the crystal grains is 60-80 mu m, and precipitated phases capable of strengthening the alloy exist in the crystal grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm. The tensile strength is 707MPa, the yield strength is 610MPa, and the elongation at break is 11.0%.
Comparative example 3-1
The same as example 3 except that the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy sheet was usedWherein Sc is 0.4-0.5 percent and Zr is 0.3-0.4 percent. The same subsequent heat treatment process is adopted. Through detection, the GP zone and eta' phase in the crystal grain of the prepared ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are reduced due to the inhibition of precipitation, and Al3The size of the (Sc, Zr) phase is increased to 30-45 nm, the number of the phases is reduced, and correspondingly obtained tensile strength is 675MPa, yield strength is 580MPa, and elongation at break is 8.5%.
Comparative examples 3 to 2
The difference from example 3 is that the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate contains 0.05-0.1% of Sc and 0.02-0.05% of Zr. The same subsequent heat treatment process is adopted. Because the addition amount of the Al and the Cu is too small, the growth of crystal grains is not inhibited in the heat treatment process, and the detection shows that the Al in the prepared ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate3The number of (Sc, Zr) phases is extremely small, the grain size is increased to 110-130 μm, the tensile strength is 610MPa, the yield strength is 525MPa, and the elongation at break is 8.0%.
Comparative examples 3 to 3
The difference from example 3 is that the alloy plate obtained in step (3) is subjected to conventional aging, the specific aging parameters are 160 ℃ for 36h, so as to obtain the Al-Zn-Mg-Cu-Sc-Zr alloy plate, and through structure observation, due to long aging time, GP zones can not be retained, so that GP zones in precipitated phases are all converted into eta ' phases, and intracrystalline precipitated phases mainly comprise eta ' phases and Al ' phases3(Sc, Zr) phase, and Al3The (Sc, Zr) phase particle size was significantly increased compared to example 3. The prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate has the tensile strength of 590MPa, the yield strength of 508MPa and the elongation after fracture of 8.8 percent.
Comparative examples 3 to 4
The difference from example 3 is that the alloy plate obtained in step (3) is subjected to two-stage aging, specifically 150 ℃ x 18h +160 ℃ x 18h, 1-stage low temperature and 2-stage high temperature, so that the high-temperature aging time is shortened, and the prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate has an intragranular precipitated phase structure, although including GP zones, eta' phase and Al phase3(Sc, Zr) phase, but each precipitated phase is relatively larger in size, particularly Al3The (Sc, Zr) phase has larger size which is more than 20nm, the performance data are that the tensile strength is 650MPa, the yield strength is 578MPa, and the elongation after fracture is7.9％。
Comparative examples 3 to 5
The difference from example 3 is that the regression re-aging process parameters adopted by the alloy plate obtained in step (3) are as follows: 150 ℃ multiplied by 18h +180 ℃ multiplied by 1h +160 ℃ multiplied by 18h, and the large-size precipitated phase redissolution effect is poor due to the fact that the prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate is too low in regression temperature. The GP zone, eta' phase and Al of the intragranular precipitated phase in the structure3The (Sc, Zr) phase was slightly reduced in size but still large, and a small amount of grain boundary did not precipitate, and the performance data was 660MPa in tensile strength, 582MPa in yield strength, and 8.2% in elongation after fracture.
Comparative examples 3 to 6
The difference from example 3 is that the bloom temperature in step (2) is 460 ℃, the tensile strength of the prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate is 672MPa, the yield strength is 594MPa, the elongation after fracture is 7.5%, and the scanning electron microscope image of the alloy tensile fracture is shown in FIG. 1.
Comparative examples 3 to 7
The difference from example 3 is that the bloom temperature in step (2) is 520 ℃, the tensile strength of the prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate is 660MPa, the yield strength is 587MPa, the elongation after fracture is 8.6%, and the scanning electron microscope image of the alloy tensile fracture is shown in FIG. 3.
As can be seen from the scanning electron microscope images of the three alloy tensile fractures shown in fig. 1-3, when the blooming temperature is 460 ℃, the tensile fracture of the alloy is mainly crystal-sugar-shaped fracture, the crystal fracture characteristic is obvious, and at the same time, the alloy has a small number of small and shallow pits, the plasticity of the alloy is relatively lowest, when the blooming temperature is 490 ℃, the tensile fracture of the alloy is mainly deeper pits, which shows that the plasticity of the alloy is relatively optimal with the ductile fracture characteristic, when the blooming temperature is increased to 520 ℃, the number of pits on the tensile fracture of the alloy is reduced, the crystal-sugar-shaped fracture is increased, the ductile-brittle mixed fracture of the alloy is caused, and the plasticity of the alloy is reduced. Therefore, the plasticity of the alloy is improved most obviously under the selection of the initial rolling temperature of 490 ℃.
Comparative examples 3 to 8
The difference from example 3 is that, in step (2), the first pass reduction was 35%, the produced Al-Zn-Mg-Cu-Sc-Zr alloy sheet cracked to various degrees, the sheet cracked as shown in FIG. 4, edge cracking occurred in the sheet, and the crack penetrated the entire sheet in the width direction.
Comparative examples 3 to 9
The difference from example 3 is that in step (2), the first pass reduction amount is 40%, and the prepared Al-Zn-Mg-Cu-Sc-Zr alloy plate cracks as shown in FIG. 5, and the head and the tail of the plate crack severely.
Comparative examples 3 to 10
The difference from example 3 is that the total rolling reduction in step (2) was carried out in 3 rolling experiments with total rolling reductions of 60%, 80% and 90%, respectively. The specific roll forming process parameters for each group are shown in table 1 below, and comparative data of alloy properties at total reduction of 60% and 80% are shown in table 2 below, wherein 2 groups are example 3.
TABLE 1
TABLE 2
The strength and plasticity of the alloy with the total reduction of 60 percent in the first group are obviously lower than those of the alloy with the total reduction of 80 percent in the second group, and the strength and plasticity of the alloy with the total reduction of 90 percent in the third group are obviously lower than those of the Al-Zn-Mg-Cu-Sc-Zr alloy plate, and the plate is found to have obvious edge cracks.
Comparative examples 3 to 11
The difference from example 3 is that the way of distributing the pass rolling reduction in step (2) is three groups of ways in the following table 3, and the rolling process strategy in group 1 adopts the larger single-pass rolling reduction as possible in the previous pass; the rolling process strategy of the group 2 adopts larger single-pass reduction in the first pass and the last pass; the rolling process strategy of group 3 used a larger single pass reduction in the subsequent pass. The rolling experiment results show that the plates in the groups 2 and 3 have edge cracks in different degrees, and the rolling process strategy adopting larger single-pass reduction in the later pass reduces the yield, so the method is not adopted.
Therefore, when the total reduction is 80%, the plate can obtain the best matching of strength and plasticity, and when the reduction of each pass is distributed, a larger single-pass reduction is required to be adopted in the previous pass as much as possible, and meanwhile, the single-pass reduction is required to be not more than 30%, so that most of the reduction tasks are completed in the previous pass, and a slightly smaller single-pass reduction is properly used in the later pass to regulate the plate shape.
TABLE 3
Claims (9)
1. An ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate is characterized by comprising the following components in percentage by mass: 6.5 to 7 percent of Zn, 1.8 to 2.3 percent of Mg, 1.9 to 2.4 percent of Cu, 0.18 to 0.22 percent of Sc, 0.08 to 0.12 percent of Zr, less than or equal to 0.1 percent of Si, less than or equal to 0.15 percent of Fe, less than or equal to 0.05 percent of Mn, less than or equal to 0.04 percent of Cr, less than or equal to 0.06 percent of Ti, and the balance of Al.
2. The ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate as recited in claim 1, wherein the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate has a tensile strength of 705MPa to 725MPa, a yield strength of 608MPa to 632MPa, and an elongation at break of 9.2% to 11.5%.
3. The ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate as claimed in claim 1, wherein the grains of the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate are equiaxial, the grain size is 60-80 μm, and precipitates capable of strengthening the alloy are present in the grains and comprise GP zones, eta' phases and Al3(Sc, Zr) phase, grain boundary non-precipitation zone in grain boundary for plasticity, Al3The (Sc, Zr) phase is fine dispersed bean-shaped particles with the particle size of 5-12 nm.
4. The process for preparing the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate as recited in claim 1, comprising the steps of:
(1) smelting and pouring the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy components to obtain an alloy casting blank;
(2) carrying out heat preservation on the alloy casting blank at the temperature of 490-510 ℃ for 1-3h, and then carrying out hot rolling, wherein the initial rolling temperature is 480-490 ℃, and the final rolling temperature is 440-450 ℃ to obtain an alloy plate; wherein the rolling pass is 5-6 passes, the total reduction is 73.33-80%, and the single-pass reduction is 20-30%;
(3) carrying out heat treatment on the alloy plate, wherein the heat treatment comprises solution treatment and regression re-aging treatment to prepare the ultrahigh-strength Al-Zn-Mg-Cu-Sc-Zr alloy plate, and the solution treatment process parameters are (480-:
(140-160℃)×(17-19h)+(190-210℃)×(0.5-1.5h)+(150-170℃)×(17-19h)。
5. the process for preparing the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate according to claim 4, wherein in the step (1), the alloy smelting temperature is 730-740 ℃; the Zn is added in a pure Zn form, the Mg is added in a pure Mg form, the Cu is added in a pure Cu form, the Sc is added in an Al-2% Sc master alloy form, the Zr is added in an Al-5% Zr master alloy form, and the charging materials are added in the following sequence: pure Al, Al-5% Zr master alloy, Al-2% Sc master alloy, pure Cu, pure Zn and pure Mg; stirring the melt while adding pure Zn; the melt was stirred while pure Mg was added.
6. The process for preparing the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate according to claim 4, wherein in the step (1), the pouring temperature is 720 ℃ to 730 ℃.
7. The process for preparing an ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy sheet as claimed in claim 4, wherein in the step (2), the rolling speed is 0.5-2.5 m/s.
8. The preparation process of the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate according to claim 4, wherein in the step (2), the 1 st pass reduction is 30%, and when the rolling pass is 5 passes, the single-pass reduction value sequence is that the 1 st pass is more than or equal to the 2 nd pass, more than or equal to the 3 rd pass, more than or equal to the 4 th pass, more than or equal to the 5 th pass; when the rolling pass is 6 passes, the single-pass reduction magnitude sequence is that the 1 st pass is more than or equal to the 2 nd pass, more than or equal to the 3 rd pass, more than or equal to the 4 th pass, more than or equal to the 5 th pass, more than or equal to the 6 th pass.
9. The process for preparing the ultra-high strength Al-Zn-Mg-Cu-Sc-Zr alloy plate according to claim 4, wherein in the step (2), the thickness of the alloy plate is 6mm to 8 mm.
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