CN111172422A - Preparation method of aluminum oxide dispersion strengthening copper-based composite material - Google Patents
Preparation method of aluminum oxide dispersion strengthening copper-based composite material Download PDFInfo
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- CN111172422A CN111172422A CN202010070275.8A CN202010070275A CN111172422A CN 111172422 A CN111172422 A CN 111172422A CN 202010070275 A CN202010070275 A CN 202010070275A CN 111172422 A CN111172422 A CN 111172422A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000010949 copper Substances 0.000 title claims abstract description 60
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000006185 dispersion Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims description 9
- 238000005728 strengthening Methods 0.000 title claims description 5
- 239000000956 alloy Substances 0.000 claims abstract description 84
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 82
- 239000000843 powder Substances 0.000 claims abstract description 57
- 239000003610 charcoal Substances 0.000 claims abstract description 35
- 238000005520 cutting process Methods 0.000 claims abstract description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005266 casting Methods 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 230000000630 rising effect Effects 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 abstract description 10
- 238000005242 forging Methods 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 10
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 229910002804 graphite Inorganic materials 0.000 description 18
- 239000010439 graphite Substances 0.000 description 18
- 229910000881 Cu alloy Inorganic materials 0.000 description 16
- 239000000243 solution Substances 0.000 description 10
- 239000004927 clay Substances 0.000 description 9
- 238000010892 electric spark Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- UNRNJMFGIMDYKL-UHFFFAOYSA-N aluminum copper oxygen(2-) Chemical compound [O-2].[Al+3].[Cu+2] UNRNJMFGIMDYKL-UHFFFAOYSA-N 0.000 description 1
- -1 and the like Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000581 reactive spray deposition Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- Engineering & Computer Science (AREA)
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- Metallurgy (AREA)
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Abstract
① A ① process ① for ① preparing ① the ① dispersion ① - ① strengthened ① copper ① - ① base ① composite ① material ① of ① alumina ① includes ① such ① steps ① as ① preparing ① mould ①, ① mixing ① with ① copper ① powder ① and ① Al ① powder ①2O3putting pure copper and water charcoal into a crucible, smelting in atmospheric environment, heating, adding dehydrated charcoal again to reduce the burning loss of alloy, keeping the temperature to obtain copper liquid, then putting the pressed blank powder into molten copper liquid, simultaneously opening an electromagnetic stirring device, and then pouring the alloy copper liquidcasting, cooling, taking out to obtain alloy cast ingot, cutting, rotary forging and stress annealing.
Description
Technical Field
The invention relates to a preparation method of a copper-based composite material, belonging to the technical field of copper alloys.
Background
Copper and copper alloy are widely applied to national industry due to good mechanical and electrical properties, but with the development of high-tech industry, especially the rapid development of electronic industry, the demand for copper alloy will be greater and greater, and the properties of traditional copper alloy can not meet the requirements, so the development and research of high-strength, high-conductivity and high-softening resistance copper alloy are very popular. Therefore, in recent years, copper alloy materials having excellent mechanical and electrical properties have been developed and have been greatly developed in various countries throughout the world. The aluminum oxide copper-based composite material is different in military projection, can simultaneously play the synergistic effect of a matrix and a reinforced material, has great design freedom, can enable the electrical conductivity of the material to be well matched with the strength or other properties of the material, is widely applied to high-tech fields such as metal casting, electronic information, electric vacuum devices, high-voltage switches, resistance welding electrodes in industries such as high-speed electrified railway equipment and automobile manufacturing, high-thrust rocket engine linings, crystallizers, bow nets and the like, and becomes one of key materials adapting to national economic development of new era.
At present, the preparation method of the alumina copper-based composite material mainly comprises 8 methods:
(1) the powder metallurgy method has mature process and good material performance, but has complex production process, high cost and low production efficiency, and simultaneously, the interface of the composite material is easy to be polluted and the interface reaction is serious.
(2) Copper-based composite material Al prepared by mechanical alloying method2O3The particles are distributed more uniformly, but the obtained composite powder is easy to be polluted, the product has larger crystal grains, and the performance is difficult to be further improved.
(3) The composite electrodeposition method does not need conditions such as high temperature and high pressure, and has simple preparation process, low cost and good component controllability. But the uniform and stable suspension of the particles in the plating solution is not easy to control, and Al in the product2O3The content and the size of the composite article are limited.
(4) The equipment and the process of the hybrid casting method are relatively simple, but the method is easy to involve partial gas, and the material property is low.
(5) Al prepared by coprecipitation method2O3The dispersed copper composite powder is affected by the reduction process and the purity of raw materials, and the performance of a sintered product is lower.
(6) The sol-gel method has complex process route and is not suitable for mass production, and the method for preparing Al at present2O3There have been few reports of dispersion-strengthened copper-based composites.
(7) The reactive spray deposition method integrates the advantages of powder metallurgy and stirring casting, overcomes the defects of high oxygen content of a matrix of a composite material product, serious interface reaction and the like, and produces the composite material with higher performance.
(8) Al in fine dispersion distribution can be obtained by internal oxidation method2O3The particle and the material have good performance, but the oxygen content required by the reaction is difficult to control, the production cost is high, the process is complicated, the influence factors are more, and the industrial production process parameters are not very clear.
The alumina copper-based composite material prepared by the method can improve the comprehensive performance of the material, but the preparation process is more complicated, so that the requirement on test equipment is higher, and the production cost is relatively high; or the preparation process is simple, but the performance of the obtained material is general, so that the realization of industrial production has some problems. The difficulty of the traditional casting method with lower cost is that the alumina particles have small density and poor wettability with the copper matrix, and the like, and alloy materials with uniformly dispersed strengthening phases are difficult to obtain.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an alumina dispersion strengthened copper-based composite material with simple working procedures and high strength and high temperature stability of the obtained material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
compared with the prior art, the invention has the advantages that: the preparation method of the aluminum oxide dispersion strengthening copper-based composite material is characterized by comprising the following steps of:
firstly, preparing a die, pure copper powder and Al2O3The mass ratio of the powder is about 2: 1-4: 1, the powder is placed in a grinder to be fully ground, and the uniformly mixed aluminum oxide and copper powder are filled into a die and pressed into blank powder;
② putting pure copper and water charcoal into the crucible, pure copper and Al2O3The mass ratio of the powder is 98:1, smelting is carried out in an atmospheric environment, dehydrated charcoal is added again when the powder is heated to 1090-1110 ℃, the burning loss of the alloy is reduced, the copper liquid is obtained after heat preservation, then the pressed blank powder is placed into the molten copper liquid, an electromagnetic stirring device is opened at the same time, the electromagnetic stirring frequency is controlled to be 20-35 HZ, the current is 70-100A, the heat preservation is carried out for 25-35 s, then the alloy copper liquid is cast, the casting speed is controlled to be 3-4 mm/s, the rising speed of the alloy liquid in a mold is 2-3.5 mm/s, the dispersion uniformity of the aluminum oxide powder in the casting process is ensured, and the cast ingot is taken out after being cooled to obtain an alloy cast ingot;
cutting, namely cutting the alloy ingot into an alloy rod material;
④, performing rotary swaging treatment, namely performing rotary swaging on the alloy rod piece for at least two passes, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 70-78%;
and fifthly, stress relief annealing treatment, namely placing the alloy rod piece subjected to the rotary swaging treatment in a heat preservation furnace to respectively perform stress relief annealing treatment at the temperature of 480-520 ℃/1h, and then performing acid pickling treatment and drying.
preferably, the particle size of the pure copper powder in the step I is 40-60 nm, and the Al is2O3The particle size of the powder is 15-25 nm.
preferably, the thickness of the first addition of dehydrated charcoal in step ② is 5-10 cm.
preferably, the cutting process described in the third step is performed by a wire electric discharge machine.
preferably, the acid washing treatment in the fifth step adopts 12 weight percent nitric acid aqueous solution.
(1) Al prepared by the invention2O3The casting method of the copper-based composite material adopts atmospheric melting, and is relative to Al2O3Other preparation methods of the copper-based composite material have simple working procedures and low cost. The Al is achieved by controlling the electromagnetic stirring frequency and current, the casting speed and the casting temperature2O3The particles have uniform dispersibility, and the material has high strength and high-temperature stability and has the potential of industrial production.
(2) Al prepared by the invention2O3The performance parameters of the copper-based composite material are shown in Table 1. As can be seen from table 1, the composite material prepared by the present invention has very excellent high temperature mechanical properties, and maintains high conductivity and good elongation.
TABLE 1 detection results of performance parameters of alumina copper-based composite materials prepared by the present invention
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) preparing a cylindrical graphite mold with a height of 250mm and an inner diameter of60 mm; 100g of pure copper powder (particle diameter 50nm, purity 99.9 wt.%), 50gAl were prepared2O3The powder (particle diameter 15nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of a dehydrated charcoal covering layer is about 5 cm), smelting in an atmospheric environment, heating to 1090 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper liquid, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 20HZ, controlling the current to be 70A, preserving heat for about 25s, then casting the alloy copper liquid, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the alloy liquid in a mould to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 70%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 480 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 900MPa, the electric conductivity reaches 78% IACS, the elongation reaches 12%, and the softening temperature is 850 ℃.
Example 2:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 150g of pure copper powder (particle diameter 50nm, purity 99.9 wt.%), 50gAl were prepared2O3Grinding powder (particle diameter of 20nm and purity of 99.99 wt.%) in grinder for 1min, and mixingThe aluminum oxide and the copper powder are filled into a mold and pressed into blank powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 20HZ, controlling the current to be 85A, preserving heat for about 30s, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 77%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 500 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 906MPa, the electric conductivity reaches 77% IACS, the elongation reaches 12%, and the softening temperature is 855 ℃.
Example 3:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 100g of pure copper powder (particle diameter 50nm, purity 99.9 wt.%), 50gAl were prepared2O3The powder (particle diameter 20nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 20HZ, the current to be 100A and the heat to be about 30S, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/S, controlling the ascending speed of the molten alloy in a mold to be 2-3.5 mm/S, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, controlling the deformation amount of each pass to be 10-15% and the total deformation amount to be 75%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 500 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 921MPa, the conductivity reaches 75% IACS, the elongation reaches 11%, and the softening temperature is 870 ℃.
Example 4:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 100g of pure copper powder (particle diameter 60nm, purity 99.9 wt.%), 50gAl were prepared2O3The powder (particle diameter 20nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 30HZ, the current to be 70A and preserving heat for about 30S, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/S, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/S, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, controlling the deformation amount of each pass to be 10-15% and the total deformation amount to be 75%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 500 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 908MPa, the conductivity reaches 77% IACS, the elongation reaches 12%, and the softening temperature is 860 ℃.
Example 5:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 200g of pure copper powder (particle diameter 40nm, purity 99.9 wt.%), 50g of Al were prepared2O3The powder (particle diameter 15nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 30HZ, controlling the current to be 85A, preserving heat for about 30S, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/S, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/S, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 78%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 500 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 924MPa, the conductivity reaches 75% IACS, the elongation reaches 11%, and the softening temperature is 865 ℃.
Example 6:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 200g of pure copper powder (particle diameter 40nm, purity 99.9 wt.%), 50g of Al were prepared2O3The powder (particle diameter 15nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 10 cm), smelting in an atmospheric environment, heating to 1110 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper liquid, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 30HZ, controlling the current to be 100A, preserving heat for about 35s, then casting the alloy copper liquid, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the alloy liquid in a mould to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 78%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 520 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 940MPa, the conductivity reaches 73% IACS, the elongation reaches 10%, and the softening temperature is 890 ℃.
Example 7:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 150g of pure copper powder (particle diameter 60nm, purity 99.9 wt.%), 50g of Al were prepared2O3The powder (particle diameter 25nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 35HZ, controlling the current to be 70A, preserving heat for about 25s, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, controlling the deformation amount of each pass to be 10-15% and controlling the total deformation amount to be 72%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 480 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 932MPa, the electric conductivity reaches 74% IACS, the elongation reaches 10%, and the softening temperature is 870 ℃.
Example 8:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 100g of pure copper powder (particle diameter 50nm, purity 99.9 wt.%), 50gAl were prepared2O3The powder (particle diameter 15nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 5 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 35HZ, controlling the current to be 85A, preserving heat for about 30s, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, controlling the deformation amount of each pass to be 10-15% and the total deformation amount to be 75%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 500 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 940MPa, the conductivity reaches 73% IACS, the elongation reaches 10%, and the softening temperature is 890 ℃.
Example 9:
(1) preparing a cylindrical graphite die, wherein the die height is 250mm, and the inner diameter is 60 mm; 100g of pure copper powder (particle diameter 50nm, purity 99.9 wt.%), 50gAl were prepared2O3The powder (particle diameter 20nm, purity 99.99 wt.%) was ground in a grinder for 1min, and the uniformly mixed alumina and copper powder were charged into a mold and pressed into a green powder.
(2) Putting 4.9Kg of pure copper rod (99.99 wt.%), sufficient dehydrated charcoal into a graphite clay crucible (the thickness of the covering layer of the dehydrated charcoal is about 8 cm), smelting in an atmospheric environment, heating to 1100 ℃, adding the dehydrated charcoal again, reducing the burning loss of the alloy, preserving heat for 2min, then putting the pressed blank powder into molten copper, simultaneously opening an electromagnetic stirring device, strictly controlling the electromagnetic stirring frequency to be 35HZ, controlling the current to be 100A, preserving heat for about 30s, then casting the molten alloy copper, controlling the casting speed to be 3.5mm/s, controlling the rising speed of the molten alloy in a mold to be 2-3.5 mm/s, so as to ensure the dispersion uniformity of the alumina powder in the casting process, and taking out the cast ingot after cooling.
(2) Cutting treatment: cutting the alloy ingot obtained in the step (1) into alloy rod materials with phi of 20mm by adopting an electric spark wire cutting machine tool;
(3) and (3) rotary swaging treatment: performing multi-pass rotary forging on the alloy rod piece obtained in the step (2) until phi is 10mm, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 78%;
(4) stress relief annealing treatment: and (4) placing the alloy rod obtained in the step (3) in a heat preservation furnace, respectively performing stress relief annealing treatment at 480 ℃/1h, then performing acid washing treatment (acid washing solution is 12% nitric acid aqueous solution), and drying.
(5) Finally, the tensile strength of the obtained copper alloy rod reaches 938MPa, the electric conductivity reaches 73% IACS, the elongation reaches 10%, and the softening temperature is 885 ℃.
Claims (5)
1. The preparation method of the aluminum oxide dispersion strengthening copper-based composite material is characterized by comprising the following steps of:
firstly, preparing a die, pure copper powder and Al2O3The mass ratio of the powder is about 2: 1-4: 1, the powder is placed in a grinder to be fully ground, and the uniformly mixed aluminum oxide and copper powder are filled into a die and pressed into blank powder;
② putting pure copper and water charcoal into the crucible, pure copper and Al2O3The mass ratio of the powder is 98:1, smelting is carried out in an atmospheric environment, dehydrated charcoal is added again when the powder is heated to 1090-1110 ℃, the burning loss of the alloy is reduced, the copper liquid is obtained after heat preservation, then the pressed blank powder is placed into the molten copper liquid, an electromagnetic stirring device is opened at the same time, the electromagnetic stirring frequency is controlled to be 20-35 HZ, the current is 70-100A, the heat preservation is carried out for 25-35 s, then the alloy copper liquid is cast, the casting speed is controlled to be 3-4 mm/s, the rising speed of the alloy liquid in a mold is 2-3.5 mm/s, the dispersion uniformity of the aluminum oxide powder in the casting process is ensured, and the cast ingot is taken out after being cooled to obtain an alloy cast ingot;
cutting, namely cutting the alloy ingot into an alloy rod material;
④, performing rotary swaging treatment, namely performing rotary swaging on the alloy rod piece for at least two passes, wherein the deformation amount of each pass is controlled to be 10-15%, and the total deformation amount is 70-78%;
and fifthly, stress relief annealing treatment, namely placing the alloy rod piece subjected to the rotary swaging treatment in a heat preservation furnace to respectively perform stress relief annealing treatment at the temperature of 480-520 ℃/1h, and then performing acid pickling treatment and drying.
2. the method according to claim 1, wherein the pure copper powder in step ① has a particle size of 40 to 60nm, and the Al is2O3The particle size of the powder is 15-25 nm.
3. the method according to claim 1, wherein the first addition of dehydrated charcoal in the second step has a thickness of 5 to 10 cm.
4. the method according to claim 1, wherein the cutting process in the third step is performed by a wire electric discharge machine.
5. the method according to claim 1, wherein the pickling process in the fifth step is performed with a 12 wt% nitric acid aqueous solution.
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| CN111957755A (en) * | 2020-07-20 | 2020-11-20 | 华东交通大学 | Drawing process for dispersion copper alloy |
| CN111996405A (en) * | 2020-08-22 | 2020-11-27 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
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| CN103343246A (en) * | 2013-07-03 | 2013-10-09 | 上海大学 | Preparation method of long-size dispersion strengthening copper-based composite material and casting device thereof |
| CN104532051A (en) * | 2014-11-28 | 2015-04-22 | 付亚波 | Diffusion-strengthened copper prepared by nano particle stirring method and preparation method thereof |
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| CN103343246A (en) * | 2013-07-03 | 2013-10-09 | 上海大学 | Preparation method of long-size dispersion strengthening copper-based composite material and casting device thereof |
| CN104532051A (en) * | 2014-11-28 | 2015-04-22 | 付亚波 | Diffusion-strengthened copper prepared by nano particle stirring method and preparation method thereof |
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| CN111957755A (en) * | 2020-07-20 | 2020-11-20 | 华东交通大学 | Drawing process for dispersion copper alloy |
| CN111957755B (en) * | 2020-07-20 | 2022-01-11 | 华东交通大学 | Drawing process for dispersion copper alloy |
| CN111996405A (en) * | 2020-08-22 | 2020-11-27 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
| CN111996405B (en) * | 2020-08-22 | 2021-12-31 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
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