CN116179913A - Al-Cu-Mg-Ag-Mn heat-resistant alloy and preparation method thereof - Google Patents
Al-Cu-Mg-Ag-Mn heat-resistant alloy and preparation method thereof Download PDFInfo
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- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
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- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/057—Changing 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 copper as the next major constituent
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Abstract
An Al-Cu-Mg-Ag-Mn heat-resistant alloy and a preparation method thereof, wherein the alloy contains the following elements in percentage by mass: cu:4.8 to 6.4 percent of Mg:0.4 to 0.8 percent, ag:0.2 to 1.2 percent, mn:0.2 to 0.8 percent, ti:0 to 0.2 percent, mo:0 to 0.2 percent, cr:0 to 0.2 percent; the balance being Al, and the sum of the mass percentages of Mo and Cr being 0.2%. The preparation method comprises the following steps: smelting and casting, namely performing two-stage homogenizing annealing on the cast ingot at 400+/-20 ℃ × (8-16) h+515+/-15 ℃ × (12-36) h; then hot rolling the slab with the thickness of 20-25 mm to 5mm at the temperature of 450-480 ℃; annealing for 1-4 h at 450-480 ℃, and then cooling to 2mm; finally, after solid solution is carried out for 1 to 6 hours at 500 to 550 ℃, aging is carried out for 8 to 16 hours at 150 to 180 ℃. The prepared alloy has higher tensile strength and yield strength under the conditions of room temperature stretching and high temperature stretching at 250 ℃; and the sample is exposed for 100-500 hours at 200-250 ℃ for a long time, the alloy still keeps higher strength, and the alloy has good thermal stability.
Description
Technical Field
The invention relates to an Al-Cu-Mg-Ag-Mn heat-resistant alloy and a preparation method thereof, belonging to the technical field of aluminum alloy.
Background
With the rapid development of the national defense industry and the aviation industry, higher requirements are put on the heat-resistant aluminum alloy, for example, when the speed of a supersonic aircraft is increased to Mach 2-4, the temperature of the aircraft skin reaches 150-250 ℃, the aluminum alloy skin is easy to soften under the extreme condition for a long time, and the strength is obviously reduced. Therefore, development of a novel heat-resistant aluminum alloy capable of being used for a long time at 200-250 ℃ is a problem to be solved urgently.
The research shows that Ag can change the aging precipitation sequence in the Al-Cu-Mg alloy with high Cu/Mg content, precipitates uniform and fine omega heat-resistant phase, has more excellent coarsening resistance compared with theta' phase, and can exist for a long time below 200 ℃ without aggregation and growth. In addition, although the addition of Ag significantly improves the high temperature strength of al—cu—mg alloys, the decrease in strength is affected by the strengthening phase coarsening, and also the grain boundary sliding and the softening of the matrix due to the grain coarsening are important factors. Therefore, in order to further improve the heat resistance of al—cu—mg—ag alloys, two main approaches are currently adopted:
first, fine grain strengthening: i.e. by refining the grains to increase the strength of the alloy, but for conventional machining it is difficult to obtain grains with a size of less than 10 μm, the performance improvement is not significant. In recent years, there has been a great deal of attention to obtaining sufficiently fine grains to improve the strength of alloys by large plastic deformation. CN101876041a discloses a method for preparing an Al-Cu-Mg-Ag superfine crystal heat-resistant aluminum alloy, which improves the heat resistance of the Al-Cu-Mg-Ag alloy in a superfine crystal strengthening manner by performing hot extrusion-solution quenching-constant diameter angular extrusion-aging treatment on the homogenized cast ingot. The mode obviously improves the high-temperature strength of the alloy, but has poor plasticity, and the coarsening of crystal grains inevitably occurs at high temperature, so that the structure stability of the nanocrystalline alloy is poor, and once the crystal grains grow up, the nanocrystalline alloy is converted into a general coarse-grain structure, and the excellent performance of the nanocrystalline alloy is lost.
Secondly, microalloying, namely refining alloy grains by adding rare earth elements such as Er, ce and the like, introducing trace transition elements such as Mn, zr and the like, and adopting a proper homogenization system to promote formation of fine dispersion phases which are coherent or semi-coherent with a matrix, so that the dispersion strengthening effect can be achieved; they can also inhibit recrystallization, pinning of grain boundaries can effectively hinder sliding of grain boundaries at high temperatures, stabilizing grain size. CN105525234a discloses a method for testing the influence of solid solution aging treatment on the performance of Al-Cu-Mg-Ag alloys containing Zr, mn, but the study does not relate to the formation of dispersed phases and the strengthening mechanism thereof; CN110724865a discloses a method for preparing an Al-Cu-Mg-Ag-Si-Sc heat-resistant aluminum alloy, wherein the synergistic effect of Sc and Si elements is exerted, so that Si and Sc elements can be biased around a precipitated phase at a lower aging temperature, coarsening of the precipitated phase is inhibited, so that the alloy has higher strength and heat-resistant effect, however Sc and Si do not have the effect of enhancing heat stability for a low Cu Al-Cu-Mg-Ag alloy. Because the diffusion rate of Mn, sc, zr and other elements is low, the equilibrium distribution coefficient K is used in the heat treatment process 0 The difference in (a) leads to the formation of a precipitate-free region and a sparse region within the crystal, and the distribution is extremely uneven. Therefore, obtaining a uniform, fine, high number density of dispersed phases is one of the effective ways to improve the high temperature thermal stability of the alloy. However, little research has been done on how to obtain uniform, fine and high number density dispersed phases of the Al-Cu-Mg-Ag-Mn system.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide an Al-Cu-Mg-Ag-Mn heat-resistant alloy and a preparation method thereof, wherein the microalloying elements are mutually cooperated to promote the number density to be 10.3/mu m by microalloying Mo and Cr and improving a homogenization system, a deformation processing technology and a solid solution and aging heat treatment system 2 Spherical Al with diameter of 86.2 + -5 nm and uniform distribution 7 (Cr, mn) and Al 6 The (Fe, mn, mo) dispersed phase is separated out to improve the dispersion strengthening effect and the high-temperature heat stability of the Al-Cu-Mg-Ag-Mn heat-resistant alloy.
The invention relates to an Al-Cu-Mg-Ag-Mn heat-resistant alloy, which comprises an Al-Cu-Mg-Ag-Mn matrix and trace Mo and Cr, wherein the existence relation of the Mo and the Cr is as follows: the sum of the mass percentages of Mo and Cr is 0.2 percent.
Wherein the mass percentages of the elements in the Al-Cu-Mg-Ag-Mn heat-resistant alloy are as follows:
4.8 to 6.4 percent of Cu, 0.4 to 0.8 percent of Mg, 0.2 to 1.2 percent of Ag, 0.2 to 0.8 percent of Mn, 0 to 0.2 percent of Ti, 0 to 0.2 percent of Mo and 0 to 0.2 percent of Cr, wherein the sum of the mass percentages of the Mo and the Cr is 0.2 percent, and the balance is Al and unavoidable impurities.
The Al-Cu-Mg-Ag-Mn heat-resistant alloy precipitates a rod-shaped T-Al after homogenization heat treatment 20 Cu 2 Mn 3 The disperse phase presents a B-core square structure and lattice parameterSpherical Al exhibiting pseudo-octahedral symmetry axis of rotation structure 7 (Cr, mn) and Al of rhombohedral crystal structure 6 (Fe, mn, mo) dispersed phase.
The tensile strength of the Al-Cu-Mg-Ag-Mn heat-resistant alloy stretched at room temperature is 470-510 MPa, the yield strength is 420-470 MPa, and the elongation is 9-12%; the tensile strength of high-temperature stretching at 250 ℃ is 300-340 MPa, the yield strength is 290-330 MPa, and the elongation is 15-21%.
The Al-Cu-Mg-Ag-Mn heat-resistant alloy is exposed for 100h and 500h at 200 ℃, and the measured optimal tensile strength is reduced by 11.8 percent and 19.4 percent compared with the room temperature tensile strength respectively; the heat exposure at 250 ℃ for 100h and 500h is reduced by 22.2% and 29.5%, and the heat resistance is excellent.
According to the preparation method of the Al-Cu-Mg-Ag-Mn series heat-resistant alloy, the Al-Cu-Mg-Ag-Mn series heat-resistant alloy is obtained by proportioning and casting according to the mass percentage of each element of the Al-Cu-Mg-Ag-Mn series heat-resistant alloy, and then performing two-stage homogenization, deformation processing, solid solution and aging treatment.
The method specifically comprises the following steps:
s1: casting
Preparing raw materials according to the mass percentages of all elements of the Al-Cu-Mg-Ag-Mn heat-resistant alloy, smelting, degassing, slagging off, keeping warm, standing, and casting to obtain an ingot;
s2: two-stage homogenization
According to DSC curve measured by a differential scanning calorimeter, exothermic peak corresponding to precipitation of dispersed phase is 380-420 ℃, and main second phase Al is 2 Cu has a melting endothermic peak at 530-560 ℃ and Cu is segregated according to the degree of segregation>Mg>Ag, cu segregation determines homogenization time in the case of preventing overburning;
and performing double-stage homogenization treatment on the ingot to obtain a homogenized ingot.
S3: deformation processing
Milling the surface of the homogenized cast ingot, and then carrying out hot rolling, annealing and cold rolling to obtain a rolled plate with fewer defects such as cracking and the like and better quality;
s4: solid solution and aging treatment
And carrying out solution treatment on the rolled plate, and then carrying out aging treatment to obtain the Al-Cu-Mg-Ag-Mn heat-resistant alloy.
Mo and Cr are added into the Al-Cu-Mg-Ag-Mn heat-resistant alloy, so that the stress corrosion cracking resistance of the alloy can be improved, and the hot cracking tendency at high temperature can be reduced; the trace Mo suppresses the formation of coarse insoluble phase containing Fe and improves the formability and fracture toughness of the alloy. In addition, according to its equilibrium distribution coefficient (K Mn <1,K Mo >1 and K Cr >1) Is different from rod-shaped Al 20 Cu 2 Mn 3 The dispersed phase is biased to be separated out in the interdendritic region, and the addition of Mo and Cr promotes the dispersed phase Al 6 (Fe, mn, mo) and Al 7 Cr is separated out, and the size, morphology, distribution and number density of the disperse phase are optimized to different degrees. The uniform and fine dispersed phase not only can play a role in dispersion strengthening, but also can improve the recrystallization temperature of Al-Cu-Mg-Ag-Mn heat-resistant alloy, effectively pin grain boundaries and inhibit coarsening of grains at high temperature, and play a role in high-temperature stability of the alloyTo decisive effect.
In the step S1, the specific process is as follows: melting pure aluminum at 730-750 ℃; heating to 750-780 ℃, and adding Al-Cu, al-Mn, al-Mo, al-Cr and Al-Ti intermediate alloy with higher melting point; cooling to 700-720 ℃ after full melting, adding pure Ag and pure Mg, pressing the pure Ag and the pure Mg into the melt by using a gas pressing cover to prevent burning loss, degassing hexachloroethane after the pure Ag and the pure Mg are melted, stirring, preserving heat and standing for 10min, and carrying out water-cooling copper mold casting after the element components in the melt are uniformly distributed;
in the step S2, the two-stage homogenization includes the following steps:
(1) Firstly, uniformly annealing the cast ingot at 400+/-20 ℃ for 8-16 hours, wherein the precipitation of a disperse phase is facilitated at the temperature;
(2) Then adjusting the temperature to 515+/-15 ℃, preserving the heat for 12-36 hours, and then air-cooling to room temperature;
in the step S3, the deforming process includes the following steps:
(1) Firstly, placing an ingot after homogenizing, of which the milling surface is 20-25 mm thick, at 450-480 ℃ for heat preservation for 1h to obtain a slab with the thickness of 20-25 mm;
(2) Hot rolling a slab with the thickness of 20-25 mm to 5mm, wherein the total reduction is 70-80%, and the processing passes are 6-8 times, so as to obtain a hot rolled plate; during hot rolling, the temperature of the cast ingot is kept above 400 ℃, so that good processing performance during deformation is ensured;
further, a slab with a thickness of 20-25 mm was hot rolled to 5mm using a two-roll hot rolling tester.
(3) Then annealing the hot rolled plate for 1-4 hours at 450-480 ℃, eliminating work hardening, reducing deformation resistance and facilitating subsequent cold working;
(3) And (3) adopting a two-roll irreversible rolling mill to perform 6-12 times of cold rolling, preferably 6-8 times of cold rolling on the annealed plate blank, wherein the total rolling reduction of the cold rolling is 30-80%, and the thickness is rolled from 5mm to 2mm, so as to obtain a deformed blank.
In the step S4, the solid solution and aging heat treatment comprises the following steps:
(1) Firstly, preserving the heat of a rolled plate at 500-550 ℃ for 1-6 h, and performing water quenching to room temperature to obtain a solid solution state alloy; preferably, the temperature is kept for 1 to 4 hours at 500 to 540 ℃; the temperature is more preferably kept at 510-530 ℃ for 1-4 hours according to the hardness and the conductivity.
(2) And then aging the solid solution state alloy at 150-180 ℃ with the optimal temperature of 165 ℃ and the time of 8-16 h to obtain the Al-Cu-Mg-Ag-Mn heat-resistant alloy.
In the step S2, it can be determined according to DSC curve that the precipitation of the dispersed phase can be promoted by carrying out the homogenization of the first stage at 400+/-20 ℃, and the dissolution of the unbalanced eutectic phase can be realized by controlling the temperature to be 515+/-15 ℃ and carrying out the homogenization of the second stage, so that the dendrite segregation is eliminated and the uniformity of the chemical components and the structure of the alloy is improved.
In the step S3, the hot rolling process in deformation processing can eliminate as-cast defects such as looseness and thinning, change as-cast structure into deformation structure, and improve the processing performance of the alloy; the annealing mainly eliminates residual stress, improves plasticity, reduces deformation resistance, and improves the non-uniformity of the structure and performance after hot rolling; the combination of deformation strengthening and solid solution and aging heat treatment generated by cold rolling can further improve the comprehensive performance of the alloy.
In the step S4, the solution treatment is carried out at high temperature and then water quenching is carried out, thereby improving the solid solubility of the strengthening elements Cu and Mg in the matrix and being beneficial to strengthening phases (theta' -Al) in the aging stage 2 Cu and Ω). In addition, a large number of dislocations and substructures exist in the deformed tissue, gradually engulf nucleation in the recovery and recrystallization stages, and form uniform and fine equiaxed crystals with the extension of time.
The Al-Cu-Mg-Ag-Mn heat-resistant alloy prepared by the invention has higher tensile strength and yield strength under room temperature stretching and 250 ℃ high temperature stretching; and the peak aging test sample is exposed for 100-500 hours at 200-250 ℃ for a long time, the alloy still keeps higher strength, and the alloy has good thermal stability.
The Al-Cu-Mg-Ag-Mn heat-resistant alloy provided by the invention has the characteristics that Mo and Cr are microalloyed, and through the two-stage homogenization, deformation processing, solid solution and aging heat treatment, the synergistic effect of Mo and Cr elements is exerted on the basis of the optimal process, so that the harm of indissolvable relative alloy mechanical properties containing Fe is reduced. By Mn,Cr and Mo equilibrium distribution coefficient (K) Mn <1,K Mo >1 and K Cr >1) Is formed by adding Mo and Cr to Al 6 (Fe, mn, mo) and Al 7 (Cr, mn) dispersed phase, eliminating rod-like T-Al 20 Cu 2 Mn 3 The dispersed phase is biased to a non-precipitation area and a precipitation sparse area caused by the precipitation of an inter-dendrite area, and the size, the morphology, the distribution and the number density of the dispersed phase are optimized to different degrees.
The uniform and fine disperse phase can play a role in dispersion strengthening, and the mechanical properties of the Al-Cu-Mg-Ag-Mn heat-resistant alloy at room temperature and high temperature are improved; and can effectively pin grain boundaries and inhibit coarsening of grains at high temperature, and plays a decisive role in high-temperature stability of the alloy.
Drawings
Fig. 1: the invention S 1 、S 2 、S 3 And S is 4 After the alloy is subjected to double-stage homogenization, the influence of Mo and Cr addition on the distribution of a disperse phase can be seen from a gold phase diagram after the alloy is corroded for 10-30s by a Kler reagent.
Fig. 2: the invention S 1 、S 2 、S 3 And S is 4 The transmission diagram of the alloy after double-stage homogenization shows Al in the alloy 20 Cu 2 Mn 3 、Al 6 (Fe, mn, mo) and Al 7 (Cr, mn) dispersed phase size and morphology changes.
Fig. 3: the invention S 1 、S 2 、S 3 And S is 4 Rod-shaped T-Al in alloy 20 Cu 2 Mn 3 Spherical Al 7 (Cr, mn) and Al 6 Statistics of the average size and number density of (Fe, mn, mo).
Fig. 4: after two-stage homogenization, the EBSD grain boundary diagram of the thermal compression shows the dynamic recrystallization condition.
Fig. 5: the invention S 1 、S 2 、S 3 And S is 4 Room temperature elongation curve of the alloy.
Fig. 6: the invention S 1 、S 2 、S 3 And S is 4 High temperature elongation curve of the alloy at 250 ℃.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
The test methods described in the following examples, unless otherwise specified, are all conventional; the reagents and materials, unless otherwise specified, are commercially available.
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1:
alloy compositions were prepared according to the following Table 1, and prepared using a graphite crucible and a water-cooled copper mold, using pure aluminum, pure magnesium, pure silver, and Al-Cu, al-Mn, al-Ti, al-Mo, and Al-Cr intermediate alloys as raw materials. Melting an aluminum ingot at the melting temperature of 730-750 ℃, heating to 750-780 ℃, adding Al-Cu, al-Mn, al-Mo, al-Ti and Al-Cr intermediate alloy, fully melting, reducing the temperature of the melt to 700-720 ℃, adding pure magnesium and pure silver, degassing with hexachloroethane after the melting, stirring, keeping the temperature and standing for 10min, and carrying out water-cooling copper mold casting after the components of each element in the melt are uniformly distributed. The actual composition of the prepared 4 groups of Al-Cu-Mg-Ag-Mn heat-resistant alloys was measured by a spectrometer and shown in Table 1.
TABLE 1 actual alloy composition
Embodiment case 2: for S in embodiment 1 1 The as-cast alloy is subjected to two-stage homogenization treatment of 400 ℃ multiplied by 12h and 515 ℃ multiplied by 24h, air-cooled to room temperature, a part of the homogenized sample is cut off, the sample is ground and polished by sand paper, and is put into a Kler reagent to be corroded for 10-30s, and the dispersion phase distribution, the size and the number density are shown in figures 1, 2 and 3. It can be seen that the rod-shaped T-Al 20 Cu 2 Mn 3 The dispersed phase segregates to dendrites, so that a large number of non-dispersed precipitation zones (DFZ) exist in the crystals, the DFZ area is 25-35%, and the T-Al 20 Cu 2 Mn 3 Length of 275.4.+ -. 9.5nm, average number density of 3.5/. Mu.m 2 ;500℃-0.01s -1 The 60% heat-compressed high-flux bipyramid sample was subjected to 400 ℃. Times.12h+515 ℃. Times.24 h treatment, and the EBSD grain boundary diagram of the core is shown in FIG. 4. The ratio of the medium angle grain boundaries (LABs), medium angle grain boundaries (MLABs) and large angle grain boundaries (HABs) in the grain boundary orientation differences was 37.52%,6.25% and 24.19%, respectively. Description S 1 The alloy only precipitates the T-Al with larger size and lower number density in the homogenization stage 20 Cu 2 Mn 3 The dispersion phase has larger DFZ area, the dispersion phase is extremely unevenly distributed, and the recrystallization inhibition effect in the thermal compression process is not obvious.
Embodiment 3: for S in embodiment 1 2 The as-cast alloy is subjected to two-stage homogenization treatment of 400 ℃ multiplied by 12h and 515 ℃ multiplied by 24h, air-cooled to room temperature, a part of the homogenized sample is cut off, the sample is ground and polished by sand paper, and is put into a Kler reagent to be corroded for 10-30s, and the dispersion phase distribution, the size and the number density are shown in figures 1, 2 and 3. It can be seen that the DFZ area in the crystal is obviously reduced, the area is 15-25%, and the T-Al 20 Cu 2 Mn 3 The length of the dispersed phase is 156.5+/-8.1 nm, and the average number density is 7.6/mu m 2 The method comprises the steps of carrying out a first treatment on the surface of the In addition to T-Al 20 Cu 2 Mn 3 In addition, spherical Al is precipitated 7 (Cr, mn) and Al 6 (Fe, mn, mo) dispersed phase with diameter of 127.6+ -3.2 nm and average number density of 5.6/. Mu.m 2 。500℃-0.01s -1 The 60% heat-compressed high-flux bipyramid sample was subjected to 400 ℃. Times.12h+515 ℃. Times.24 h treatment, and the EBSD grain boundary diagram of the core is shown in FIG. 4. The ratio of the medium angle grain boundaries (LABs), medium angle grain boundaries (MLABs) and large angle grain boundaries (HABs) in the grain boundary orientation differences was 42.72%,6.51% and 18.55%, respectively. Indicating that the addition of 0.15wt% Cr and 0.05wt% Mo reduces T-Al on average 20 Cu 2 Mn 3 43.17% length of dispersed phase, 4.1/. Mu.m increase in number density 2 DFZ is also reduced by 10%; in addition, the precipitation of the spherical dispersed phase inhibits the dislocation movement and subgrain boundary migration, so that the transformation from LABs to HABs is inhibited, and the recrystallization temperature of the alloy is increased.
Embodiment 4: for S in embodiment 1 3 As-cast stateThe alloy is subjected to two-stage homogenization treatment of 400 ℃ multiplied by 12h and 515 ℃ multiplied by 24h, air-cooled to room temperature, a part of the homogenized sample is cut, ground and polished by sand paper, and is put into a Kler reagent to be corroded for 10-30s, and the dispersion phase distribution, the size and the number density are shown in figures 1, 2 and 3. It can be seen that the area of DFZ in the crystal is larger than that of S 2 Is increased by 20 to 30 percent and T-Al 20 Cu 2 Mn 3 The length of the disperse phase is 172.7+/-6.7 nm, and the average number density is 5.0/mu m 2 ;Al 7 (Cr, mn) and Al 6 The diameter of the (Fe, mn, mo) dispersed phase is 105.4+ -2.7 nm, and the average number density is 7.7/. Mu.m 2 。500℃-0.01s -1 The 60% heat-compressed high-flux bipyramid sample was subjected to 400 ℃. Times.12h+515 ℃. Times.24 h treatment, and the EBSD grain boundary diagram of the core is shown in FIG. 4. The ratio of the medium angle grain boundaries (LABs), medium angle grain boundaries (MLABs) and large angle grain boundaries (HABs) in the grain boundary orientation differences was 44.96%,6.02% and 17.37%, respectively. Illustrating the addition of 0.10wt% Cr and 0.10wt% Mo, DFZ area vs S 2 Although the alloy is more than 5%, T-Al 20 Cu 2 Mn 3 The length of (2) is increased by 10.35%, and the number density is reduced by 2.6/. Mu.m 2 The method comprises the steps of carrying out a first treatment on the surface of the But the average diameter of the spherical dispersed phase is reduced by 22.2nm, and the number density is increased by 2.1/mu m 2 The conversion of LABs to HABs is further suppressed, and the spherical dispersed phase exhibits a more excellent recrystallization-suppressing effect than the rod-like dispersed phase.
Embodiment case 5: for S in embodiment 1 4 The as-cast alloy is subjected to two-stage homogenization treatment of 400 ℃ multiplied by 12h and 515 ℃ multiplied by 24h, air-cooled to room temperature, a part of the homogenized sample is cut off, the sample is ground and polished by sand paper, and is put into a Kler reagent to be corroded for 10-30s, and the dispersion phase distribution, the size and the number density are shown in figures 1, 2 and 3. It can be seen that as the Mo percentage increases to 0.15%, al 6 The precipitation of (Fe, mn, mo) dispersed phase to branch crystal nucleus area eliminates DFZ basically completely, and the distribution is more uniform. T-Al 20 Cu 2 Mn 3 The size of the dispersed phase is 183.5 +/-7.5 nm, and the average number density is 4.5/mu m 2 ;Al 7 (Cr, mn) and Al 6 The size of the (Fe, mn, mo) dispersed phase is 86.2+ -4.6 nm, and the average number density is 10.3/. Mu.m 2 。500℃-0.01s -1 The 60% heat-compressed high-flux bipyramid sample was subjected to 400 ℃. Times.12h+515 ℃. Times.24 h treatment, and the EBSD grain boundary diagram of the core is shown in FIG. 4. The ratio of the medium angle grain boundaries (LABs), medium angle grain boundaries (MLABs) and large angle grain boundaries (HABs) in the grain boundary orientation differences was 44.83%,5.11% and 14.75%, respectively. The addition of 0.05wt% Cr and 0.15wt% Mo promotes the uniform distribution of the dispersed phase, the DFZ is completely eliminated, the spherical dispersed phase has small size and maximum number density, the dislocation movement and subgrain boundary migration are effectively prevented, and the recrystallization inhibition effect is most obvious.
Embodiment 6: the deformation processing is carried out on the Al-Cu-Mg-Ag-Mn alloy subjected to the two-stage homogenization treatment for 4 groups of cases 2-5 at 400 ℃ multiplied by 12h+515 ℃ multiplied by 24h, and the specific process is as follows: hot rolling at 470 ℃, wherein the total deformation is 80%, the processing passes are 6 times, the hot rolled plate is annealed at 475 ℃ for 2 hours, residual stress is eliminated, cold rolling is carried out after air cooling, the total deformation is 60%, and the processing passes are 12 times; the re-solid solution aging treatment comprises the following specific processes: the cold-rolled sheet was solution-treated at 525℃and immediately water-quenched after heat preservation for 1 hour, then was subjected to aging treatment at 165℃for 8 hours, and room-temperature stretching and high-temperature stretching at 250℃were performed on 4 sets of Al-Cu-Mg-Ag-Mn, the stretching curves being shown in FIGS. 5 and 6, respectively. As can be seen from fig. 5, the addition of Cr and Mo increases the room temperature tensile strength of the alloy to varying degrees. Wherein S is 4 The alloy No. reaches the maximum strength of 505.7MPa, the yield strength is 464.9MPa, the elongation is 9.7 percent, compared with S 1 The tensile strength and the yield strength of the alloy number are respectively improved by 27.8MPa and 35.3MPa, and the elongation rate is not greatly changed. As can be seen from fig. 6, the addition of Cr and Mo improved the high temperature tensile strength of the alloy to different extents. Wherein S is 4 The high-temperature strength of the alloy No. reaches the maximum 338.7MPa, the yield strength is 329.6MPa, and the elongation is 19.0 percent, compared with S 1 The tensile strength and the yield strength of the alloy number are respectively improved by 28.0MPa and 28.1MPa.
Embodiment 7: for example 6, the two-stage homogenization, hot rolling and cold rolling at 400 ℃ and 12h+515 ℃ and 24h, and solid solution at 525 ℃ and aging at 165 ℃ for 8h were performed 1 The sheet material is subjected to a heat exposure test, and the specific steps are as follows: performing heat exposure treatment at 200deg.C and 250deg.C for 100h and 500h, and performing mechanical propertiesThe results of the test are shown in Table 2.
Embodiment case 8: for example 4, the two-stage homogenization, hot rolling and cold rolling were performed at 400 ℃ by 12h+515 ℃ by 24h, and solid solution at 525 ℃ for 1h and aging at 165 ℃ for 8h 2 The sheet material is subjected to a heat exposure test, and the specific steps are as follows: the heat exposure treatment was performed at 200℃and 250℃for 100 hours and 500 hours, and the mechanical properties were tested, and the results are shown in Table 3.
Embodiment case 9: for example 4, the two-stage homogenization, hot rolling and cold rolling were performed at 400 ℃ by 12h+515 ℃ by 24h, and solid solution at 525 ℃ for 1h and aging at 165 ℃ for 8h 3 The sheet material is subjected to a heat exposure test, and the specific steps are as follows: the heat exposure treatment was performed at 200℃and 250℃for 100 hours and 500 hours, and the mechanical properties were tested, and the results are shown in Table 4.
Embodiment case 10: for example 4, the two-stage homogenization, hot rolling and cold rolling were performed at 400 ℃ by 12h+515 ℃ by 24h, and solid solution at 525 ℃ for 1h and aging at 165 ℃ for 8h 4 The sheet material is subjected to a heat exposure test, and the specific steps are as follows: the heat exposure treatment was performed at 200℃and 250℃for 100 hours and 500 hours, and the mechanical properties were tested, and the results are shown in Table 5.
TABLE 2
TABLE 3 Table 3
TABLE 4 Table 4
TABLE 5
Claims (10)
1. An Al-Cu-Mg-Ag-Mn heat resistant alloy, characterized in that: the Al-Cu-Mg-Ag-Mn heat-resistant alloy comprises an Al-Cu-Mg-Ag-Mn matrix and trace Mo and Cr, wherein the existence relation of the Mo and the Cr is as follows: the sum of the mass percentages of Mo and Cr is 0.2 percent.
2. The Al-Cu-Mg-Ag-Mn-based heat resistant alloy according to claim 1, wherein: the Al-Cu-Mg-Ag-Mn matrix comprises the following chemical components in percentage by mass:
4.8 to 6.4 percent of Cu, 0.4 to 0.8 percent of Mg, 0.2 to 1.2 percent of Ag, 0.2 to 0.8 percent of Mn, 0 to 0.2 percent of Ti, and the balance of Al and unavoidable impurities.
3. An Al-Cu-Mg-Ag-Mn heat resistant alloy, characterized in that: micro Mo and Cr are added into an Al-Cu-Mg-Ag-Mn matrix, wherein the chemical components of the elements are as follows in percentage by mass:
4.8 to 6.4 percent of Cu, 0.4 to 0.8 percent of Mg, 0.2 to 1.2 percent of Ag, 0.2 to 0.8 percent of Mn, 0 to 0.2 percent of Ti, 0 to 0.2 percent of Mo, 0 to 0.2 percent of Cr, the sum of the mass percentages of Mo and Cr is 0.2 percent, and the balance of Al and unavoidable impurities.
4. The Al-Cu-Mg-Ag-Mn-based heat resistant alloy according to any one of claims 1 to 3, wherein: the Al-Cu-Mg-Ag-Mn heat-resistant alloy precipitates a rod-shaped T-Al after homogenization heat treatment 20 Cu 2 Mn 3 Disperse phase, B-core square structure and lattice parameterSpherical Al exhibiting pseudo-octahedral symmetry axis of rotation structure 7 (Cr, mn) and Al of rhombohedral crystal structure 6 (Fe, mn, mo) dispersed phase.
5. The Al-Cu-Mg-Ag-Mn-based heat resistant alloy according to any one of claims 1 to 3, wherein: the tensile strength of the Al-Cu-Mg-Ag-Mn heat-resistant alloy stretched at room temperature is 470-510 MPa, the yield strength is 420-470 MPa, and the elongation is 9-12%; the tensile strength of high-temperature stretching at 250 ℃ is 300-340 MPa, the yield strength is 290-330 MPa, and the elongation is 15-21%;
the Al-Cu-Mg-Ag-Mn heat-resistant alloy is exposed for 100h and 500h at 200 ℃, and the measured optimal tensile strength is reduced by 11.8 percent and 19.4 percent compared with the room temperature tensile strength respectively; the heat exposure at 250 ℃ for 100h and 500h is reduced by 22.2% and 29.5%, and the heat resistance is excellent.
6. The method for producing an Al-Cu-Mg-Ag-Mn based heat-resistant alloy according to any one of claims 1 to 3, wherein: and (3) proportioning and casting according to the mass percentages of the elements of the Al-Cu-Mg-Ag-Mn series heat-resistant alloy, and then carrying out two-stage homogenization, deformation processing, solid solution and aging treatment to obtain the Al-Cu-Mg-Ag-Mn series heat-resistant alloy.
7. The method for producing an Al-Cu-Mg-Ag-Mn series heat-resistant alloy according to claim 6, wherein: the fusion casting is as follows: firstly, melting pure Al, controlling the temperature to be 730-750 ℃, then adding Al-Cu, al-Mn, al-Ti, al-Mo and Al-Cr intermediate alloy, controlling the temperature to be 750-780 ℃, after the Al-Cu intermediate alloy is melted, controlling the melting temperature to be 700-720 ℃, adding pure Ag and pure Mg, after the Al-Cu intermediate alloy is fully melted, degassing hexachloroethane, deslagging, stirring, keeping the temperature and standing, and carrying out water-cooling copper mold casting after the melt elements are uniformly distributed.
8. The method for producing an Al-Cu-Mg-Ag-Mn series heat-resistant alloy according to claim 6, wherein: the two-stage homogenization process comprises the following steps: the first stage: preserving heat for 8-16 h at 400+/-20 ℃; and a second stage: preserving heat for 12-36 h at 515+/-15 ℃; and then air-cooling to room temperature.
9. The method for producing an Al-Cu-Mg-Ag-Mn series heat-resistant alloy according to claim 6, wherein: the deformation processing is as follows: carrying out hot rolling and cold rolling, wherein the hot rolling temperature is controlled to be 450-480 ℃, the total reduction is 70-80%, and the processing passes are 6-8 times; the intermediate annealing temperature is 450-480 ℃ and the time is 1-4 h; the total rolling reduction is 30-80%, and the processing times are 6-12.
10. The method for producing an Al-Cu-Mg-Ag-Mn series heat-resistant alloy according to claim 6, wherein: the temperature of the solution treatment is controlled at 500-550 ℃, the heat preservation time is 1-6 h, and the solution is immediately quenched after being taken out;
the temperature of the aging treatment is controlled at 150-180 ℃ and the heat preservation time is 8-16 h.
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