CN118064857A - Preparation method of fine-grain silver target - Google Patents
Preparation method of fine-grain silver target Download PDFInfo
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- CN118064857A CN118064857A CN202410199559.5A CN202410199559A CN118064857A CN 118064857 A CN118064857 A CN 118064857A CN 202410199559 A CN202410199559 A CN 202410199559A CN 118064857 A CN118064857 A CN 118064857A
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 52
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004332 silver Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005096 rolling process Methods 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000000137 annealing Methods 0.000 claims abstract description 31
- 238000003723 Smelting Methods 0.000 claims abstract description 26
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011651 chromium Substances 0.000 claims abstract description 25
- 239000010949 copper Substances 0.000 claims abstract description 25
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 20
- 238000001953 recrystallisation Methods 0.000 claims abstract description 20
- 238000001125 extrusion Methods 0.000 claims abstract description 18
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007493 shaping process Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 150000002910 rare earth metals Chemical class 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000010309 melting process Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 7
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 238000010353 genetic engineering Methods 0.000 abstract description 3
- 230000002159 abnormal effect Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 14
- 239000000956 alloy Substances 0.000 description 14
- 229910001316 Ag alloy Inorganic materials 0.000 description 8
- 239000013077 target material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
- 229910000765 intermetallic Inorganic materials 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 238000000265 homogenisation Methods 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 238000011534 incubation Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910017944 Ag—Cu Inorganic materials 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229910002530 Cu-Y Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
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Abstract
The invention provides a preparation method of a fine-grain silver target, which belongs to the technical field of metal target preparation and comprises the following steps: step one: smelting copper, silver, chromium, yttrium and other elements in a protective atmosphere to obtain a silver-copper alloy cast ingot; step two: sequentially carrying out homogenizing annealing, multipass angle extrusion, rolling, intermediate annealing and finish rolling shaping on the silver-copper alloy cast ingot obtained in the first step to obtain a silver-copper alloy rolled plate; step three: sequentially carrying out recrystallization treatment and low-temperature aging treatment on the silver-copper alloy rolled plate obtained in the second step to obtain a silver-copper alloy target; according to the invention, through the design idea of material genetic engineering and through the proportional addition of rare earth element Y and transition metal element Cr, abnormal growth of crystal grains in the recrystallization annealing process is avoided by controlling the two-stage heat treatment method after multi-pass rolling and intermediate annealing and final rolling, and uniform refinement of crystal grain structure is realized.
Description
Technical Field
The invention mainly relates to the technical field of metal target preparation, in particular to a preparation method of a fine-grain silver target.
Background
The silver target has wide application: (1) The method is mainly used for preparing high-purity silver materials such as silver foil, silver powder and the like; (2) Because silver has excellent conductivity and stability, the electronic component manufactured by using the silver target material has the advantages of high performance, long service life, low cost and the like; (3) Silver targets are important materials in the electronics industry for the manufacture of electronic components, such as integrated circuits, transistors, and displays; (4) The silver target material can also be used for manufacturing electrodes, conductive slurry and the like of the solar cell, so that the photoelectric conversion efficiency is improved and the manufacturing cost is reduced; (5) Silver targets are also widely used in the fields of jewelry, tableware, artwork and the like.
The silver target is mainly applied to preparing a silver film by magnetron sputtering, and the microstructure such as the grain size, the crystal orientation, the density and the like of the target have larger influence on the adhesiveness, the deposition rate, the photoelectric performance and the like of the magnetron sputtering film. The microstructure of the target material can be adjusted and controlled by homogenization treatment, recrystallization annealing, machining and the like. The method in which alloying is assisted by plastic deformation processing is an important way to obtain a uniform silver target structure.
The grain refinement of the silver target in the current market is mainly obtained by a rolling and recrystallization process, and the grain refinement effect of rolling is limited, so that the grain refinement of the silver target is difficult to be further refined to the grade of 20 mu m, and the technical progress of the silver target is hindered.
Disclosure of Invention
The invention mainly provides a preparation method of a fine-grain silver target material, which is used for solving the technical problems in the background technology.
The technical scheme adopted for solving the technical problems is as follows:
the preparation method of the fine-grain silver target comprises the following steps:
Step one: smelting copper, silver, chromium, yttrium and other elements in a protective atmosphere to obtain a silver-copper alloy cast ingot;
Step two: sequentially carrying out homogenizing annealing, multipass angle extrusion, rolling, intermediate annealing and finish rolling shaping on the silver-copper alloy cast ingot obtained in the first step to obtain a silver-copper alloy rolled plate;
step three: and (3) sequentially carrying out recrystallization treatment and low-temperature aging treatment on the silver-copper alloy rolled plate obtained in the step two to obtain the silver-copper alloy target.
Further, in the present invention, the smelting process in the first step specifically includes: pure silver with the purity of 99.95%, pure copper with the purity of 99.0%, pure chromium with the purity of 99.5%, and rare earth yttrium with the purity of 99.0% are weighed in proportion, and silver and rare earth yttrium are firstly put into an intermediate frequency induction crucible for smelting.
Further, in the present invention, the smelting temperature in the smelting process in the first step is controlled to 1160-1180 ℃.
Further, in the present invention, the temperature of the homogenizing annealing process in the second step is set at 800 ℃, the holding time is 2-3 hours, and then furnace cooling is performed.
Further, in the invention, the multi-pass angle extrusion process in the second step adopts a vertical downward extrusion mode, the angle is 120 degrees, the extrusion force is 10 tons, and the extrusion passes are 3.
Further, in the present invention, the rolling process in the second step specifically includes: and (3) carrying out multi-pass rolling on the cast ingot, wherein the rolling pass deformation is 30% -20% -20% in sequence.
Further, in the present invention, the temperature at the time of the intermediate annealing in the second step is 350 ℃ for 1 to 1.5 hours.
Further, in the present invention, the finishing deformation amount in the finishing shaping treatment in the second step is 10%.
Further, in the present invention, the recrystallization treatment process temperature in the third step is set at 300℃for 3 hours.
Further, in the invention, the low-temperature aging treatment process temperature in the third step is set to 250 ℃ for 1 hour.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the invention, through the design idea of material genetic engineering and through the proportional addition of rare earth element Y and transition metal element Cr, abnormal growth of crystal grains in the recrystallization annealing process is avoided by controlling the two-stage heat treatment method after multi-pass rolling and intermediate annealing and final rolling, and uniform refinement of crystal grain structure is realized.
2. In the alloy component provided by the invention, rare earth elements Y and Cu sequentially form intermetallic compounds such as Cu 7Y2、Cu4 Al, cu 6 Y and the like, and the intermetallic compounds become pinning sites for inhibiting the growth of recrystallized grains, so that the grain structure is refined. The transition metal element Cr has a great solid solution strengthening effect in silver, so that the strength is improved, and the recovery and recrystallization are weakened.
3. The invention adopts two-stage heat treatment after final rolling to respectively generate Cu 4 Y and Cu 6 Y intermetallic compounds, inhibit the growth of recrystallized grains and obtain fine and uniform grain structures.
4. The alloy composition is based on one case of material genetic engineering, and the obtained experimental result is unpredictable by conventional conjecture and has vivid innovation.
The invention will be explained in detail below with reference to the drawings and specific embodiments.
Drawings
FIG. 1 is a flow chart of a process for preparing a fine grain silver target of the present invention;
FIG. 2 is a process route diagram of the fine grain silver target of the present invention;
FIG. 3 is a ternary Ag1.5Cu-Y pseudo-binary phase diagram based on the material gene method of the present invention (by fixing the proportion of Cu, the effect of Y content on the phase composition of Ag1.5Cu alloy is predicted);
FIG. 4 is a pseudo binary phase diagram of a ternary Ag1.5Cu—Cr based material gene method of the present invention (by fixing the proportion of Cu, the effect of Cr content on the phase composition of Ag1.5Cu alloy is predicted, cr exists in a solid solution form substantially in the range of 0-2.8);
FIG. 5 is a pseudo-binary phase diagram of a quaternary Ag1.5Cu0.2Y—Cr alloy based on the material gene method of the present invention (by fixing the ratio of Ag, cu, Y, the effect of Cr content on the phase composition of Ag1.5Cu alloy is predicted).
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will be rendered by reference to the appended drawings, in which several embodiments of the invention are illustrated, but which may be embodied in different forms and are not limited to the embodiments described herein, which are, on the contrary, provided to provide a more thorough and complete disclosure of the invention.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may be present, and when an element is referred to as being "connected" to the other element, it may be directly connected to the other element or intervening elements may also be present, the terms "vertical", "horizontal", "left", "right" and the like are used herein for the purpose of illustration only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in this description of the invention are for the purpose of describing particular embodiments only and are not intended to be limiting of the invention, with the term "and/or" as used herein including any and all combinations of one or more of the associated listed items.
The preparation method of the fine-grain silver target comprises the following steps:
Step one: smelting copper, silver, chromium, yttrium and other elements in a protective atmosphere to obtain a silver-copper alloy cast ingot;
Step two: sequentially carrying out homogenizing annealing, multipass angle extrusion, rolling, intermediate annealing and finish rolling shaping on the silver-copper alloy cast ingot obtained in the first step to obtain a silver-copper alloy rolled plate;
step three: and (3) sequentially carrying out recrystallization treatment and low-temperature aging treatment on the silver-copper alloy rolled plate obtained in the step two to obtain the silver-copper alloy target.
The elements of the present invention have the following roles:
Cr element: the Cr element exists in the Ag and Cu phases mainly in the form of solid solution, and plays a role in solid solution strengthening. In addition, the solid solution of Cr element also reduces the tendency to recover and recrystallize, and inhibits grain growth. However, when the content of Cr element is higher than 2.7wt.%, elemental Cr particles are generated and increase as the relative content of Cr increases, and thus the content of Cr is set in the range of 1 to 3wt.% in the present invention.
Cu: the Cu element is the main alloy element of the Ag-Cu alloy target, and the range of the Cu element belongs to the common range.
And Y element: the element Y belongs to rare earth elements, and the addition of the element Y can form various Cu-Y intermetallic compounds which are solidified and precipitated and aged and precipitated, so that the stability of a deformed structure can be ensured, the resistance of recrystallization can be improved, and a fine and uniform target structure can be obtained.
Further, in the present invention, the smelting process in the first step specifically includes: pure silver with the purity of 99.95%, pure copper with the purity of 99.0%, pure chromium with the purity of 99.5%, and rare earth yttrium with the purity of 99.0wt.% are weighed in proportion, silver and rare earth yttrium are firstly put into an intermediate frequency induction crucible to be smelted, and the smelting temperature in the smelting process in the first step is controlled to be 1160-1180 ℃.
The temperature of the homogenizing annealing process in the second step is set at 800 ℃, the heat preservation time is 2-3 hours, and then the furnace cooling is carried out.
The multi-pass angle extrusion process in the second step adopts a vertical downward extrusion mode, wherein the angle is 120 degrees, the extrusion force is 10 tons, and the extrusion passes are 3;
It should be noted that when the number of extrusion passes is more than 3, the structure refining effect on the alloy of the invention is not great, and the refining effect is improved by about 1%, so that the extrusion passes are 3.
Further, the rolling process in the second step specifically comprises the following steps: carrying out multi-pass rolling on the cast ingot, wherein the deformation of the rolling passes is 30% -20% -20% in sequence;
It should be noted that, through the multi-pass rolling and the intermediate heat treatment, the grain structure of the material is continuously refined, and meanwhile, the phenomenon of uneven deformation and uneven structure along the normal direction of the rolled plate are avoided.
Further, the temperature in the intermediate annealing in the second step is 350 ℃ and the time is 1-1.5 hours;
by the above intermediate annealing, the recrystallization refinement of the crystal grains is realized, and the control time is controlled within 1-1.5 hours, thereby avoiding the growth of the crystal grains.
Further, in the finish rolling shaping treatment in the second step, the finish rolling deformation amount was 10%.
Further, the temperature of the recrystallization treatment process in the third step is set at 300 ℃ for 3 hours;
this step is a final heat treatment step, and a fine and uniform recrystallized structure is formed by the heat treatment.
Further, the low-temperature aging treatment process in the third step is set to 250 ℃ for 1h;
the precipitation and stabilization of the precipitated phase and further stabilization of the structure were achieved by the low-temperature aging treatment. On the other hand, the heat treatment in the low temperature section helps to eliminate residual stress and reduce dimensional deformation.
In combination with the above preparation method, in example 1, alloy compositions containing Ag, cu, Y, cr were used, the contents of which were respectively set in Cr:1 to 3 weight percent of Cu:0.5 to 1.5 weight percent, Y:0.2 to 1.2 weight percent, and the balance of Ag;
preparing a silver-copper target by smelting and combining multi-pass rolling to obtain the silver-copper target;
The preparation steps are sequentially carried out, and S1 (smelting): the preparation process comprises smelting, homogenizing annealing, multi-pass rolling, intermediate annealing, finish rolling, recrystallization treatment and low-temperature aging treatment. Specifically, the smelting process comprises the following steps: weighing 99.95% pure silver, 99.0% pure copper and 99.5% pure chromium, wherein 99.0% rare earth yttrium is weighed in proportion, and firstly putting silver and rare earth yttrium into an intermediate frequency induction crucible for smelting, wherein the smelting temperature is controlled at 1160 ℃;
S2 (multipass rolling): homogenizing annealing process: the homogenization temperature was set at 800 ℃ and the incubation time was 2-3 hours (see figure 3). The multi-pass rolling process comprises the following steps: and (3) carrying out multi-pass rolling on the cast ingot, wherein the rolling pass deformation is 30% -20% -20% in sequence. Intermediate annealing temperature: the intermediate annealing temperatures corresponding to the multi-pass rolling are respectively 350 ℃ and the time is 1-1.5 hours. And (3) finishing: the final rolling deformation is 10%, and the final rolling directly enters a recrystallization refining stage;
s3 (two-stage heat treatment): the recrystallization treatment temperature is 300 ℃ and the time is 3 hours. The temperature of the low-temperature aging treatment is 250 ℃ and the time is 1h.
The grain size of the silver alloy target material obtained in the embodiment 1 reaches 15-20 mu m.
In combination with the above preparation method, in example 2, the alloy components used include Ag, cu, and Y, and the contents of the alloy components are respectively in Cu:0.5 to 1.5 weight percent, Y:0.2 to 1.2 weight percent, and the balance of Ag;
the same preparation steps as in example 1 were sequentially carried out;
The grain size of the silver alloy target material obtained in the embodiment 2 reaches 18-25 mu m.
In combination with the above preparation method, in example 3, the alloy components used include Ag, cu, and Cr, and the contents of the alloy components are respectively set at Cr:1 to 3 weight percent of Cu:0.5 to 1.5 weight percent, and the balance of Ag;
the same preparation steps as in example 1 were sequentially carried out;
the grain size of the silver alloy target material obtained in the embodiment 2 reaches 20-28 mu m.
Comparative example 1: the alloy comprises Ag and Cu, wherein the contents of the Ag and the Cu are respectively as follows: 0.5 to 1.5 weight percent, and the balance of Ag;
preparing a silver-copper target by smelting and combining multi-pass rolling to obtain the silver-copper target;
preparing a silver-copper target by smelting and combining multi-pass rolling to obtain the silver-copper target;
S1 (smelting): the preparation process comprises smelting, homogenizing annealing, multi-pass rolling, intermediate annealing, finish rolling, recrystallization treatment and low-temperature aging treatment. Specifically, the smelting process comprises the following steps: weighing pure silver with the purity of 99.95 percent and pure copper with the purity of 99.0 percent in proportion, putting the mixture into an intermediate frequency induction crucible for smelting, and controlling the smelting temperature at 1160 ℃;
S2 (multipass rolling): homogenizing annealing process: the homogenization temperature was set at 800 ℃ and the incubation time was 2-3 hours (see figure 3). The multi-pass rolling process comprises the following steps: and (3) carrying out multi-pass rolling on the cast ingot, wherein the rolling pass deformation is 30% -20% -20% in sequence. Intermediate annealing temperature: the intermediate annealing temperatures corresponding to the multi-pass rolling are respectively 350 ℃ and the time is 1-1.5 hours. And (3) finishing: the final rolling deformation is 10%, and the final rolling directly enters a recrystallization refining stage;
s3 (single stage heat treatment): the recrystallization treatment temperature is 300 ℃ and the time is 3 hours;
The grain size of the silver alloy target material obtained in the comparative example 1 reaches 25-30 mu m.
As can be obtained by comparing the respective examples and comparative examples with fig. 3 and 4 and fig. 5, the grain size of the silver alloy target obtained in example 1 is the smallest, the grain size of the silver alloy target obtained in comparative example 1 is the smallest, and the grain size of the silver alloy target obtained in example 2 and example 3 is smaller overall than that of comparative example 1;
it can be obtained that the grain size of the silver alloy target can be effectively controlled by proportionally adding the rare earth element Y and the transition metal element Cr and controlling the two-stage heat treatment method after multi-pass rolling and intermediate annealing and final rolling.
While the invention has been described above with reference to the accompanying drawings, it will be apparent that the invention is not limited to the embodiments described above, but is intended to be within the scope of the invention, as long as such insubstantial modifications are made by the method concepts and technical solutions of the invention, or the concepts and technical solutions of the invention are applied directly to other occasions without any modifications.
Claims (10)
1. The preparation method of the fine-grain silver target is characterized by comprising the following steps of:
Step one: smelting copper, silver, chromium, yttrium and other elements in a protective atmosphere to obtain a silver-copper alloy cast ingot;
Step two: sequentially carrying out homogenizing annealing, multipass angle extrusion, rolling, intermediate annealing and finish rolling shaping on the silver-copper alloy cast ingot obtained in the first step to obtain a silver-copper alloy rolled plate;
step three: and (3) sequentially carrying out recrystallization treatment and low-temperature aging treatment on the silver-copper alloy rolled plate obtained in the step two to obtain the silver-copper alloy target.
2. The method for preparing a fine-grain silver target according to claim 1, wherein the smelting process in the first step is specifically: pure silver with the purity of 99.95%, pure copper with the purity of 99.0%, pure chromium with the purity of 99.5%, and rare earth yttrium with the purity of 99.0% are weighed in proportion, and silver and rare earth yttrium are firstly put into an intermediate frequency induction crucible for smelting.
3. The method for producing a fine-grain silver target according to claim 2, wherein the melting temperature in the melting process in the step one is controlled to 1160 ℃ to 1180 ℃.
4. The method for producing a fine-grained silver target according to claim 1, wherein the temperature of the homogenizing annealing process in the second step is set at 800 ℃, the holding time is 2-3 hours, and then furnace cooling is performed.
5. The method for preparing a fine grain silver target according to claim 1, wherein the multi-pass angle extrusion process in the second step adopts a vertical downward extrusion mode, the angle is 120 degrees, the extrusion force is 10 tons, and the extrusion passes are 3.
6. The method for preparing a fine-grain silver target according to claim 1, wherein the rolling process in the second step is specifically: and (3) carrying out multi-pass rolling on the cast ingot, wherein the rolling pass deformation is 30% -20% -20% in sequence.
7. The method for producing a fine-grained silver target according to claim 1, characterized in that the temperature at the time of the intermediate annealing in the second step is 350 ℃ for 1 to 1.5 hours.
8. The method for producing a fine-grained silver target according to claim 1, wherein the finishing deformation amount is 10% in the finishing shaping treatment in the second step.
9. The method for preparing a fine-grain silver target according to claim 1, wherein the recrystallization treatment process in the third step is set at 300 ℃ for 3 hours.
10. The method for preparing a fine-grain silver target according to claim 1, wherein the low-temperature aging treatment process in the third step is set to 250 ℃ for 1 hour.
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