CN112391550A - Preparation method of yttrium oxide dispersion strengthened copper - Google Patents
Preparation method of yttrium oxide dispersion strengthened copper Download PDFInfo
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- CN112391550A CN112391550A CN202011415658.0A CN202011415658A CN112391550A CN 112391550 A CN112391550 A CN 112391550A CN 202011415658 A CN202011415658 A CN 202011415658A CN 112391550 A CN112391550 A CN 112391550A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 89
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 38
- 239000010949 copper Substances 0.000 title claims abstract description 38
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 19
- 239000011812 mixed powder Substances 0.000 claims abstract description 19
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 230000009467 reduction Effects 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000002490 spark plasma sintering Methods 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 abstract description 8
- 230000002776 aggregation Effects 0.000 abstract description 8
- 230000002787 reinforcement Effects 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 5
- 238000004321 preservation Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- GWHUBCMJWKDESZ-UHFFFAOYSA-N [O-2].[Y+3].[Cu+2] Chemical compound [O-2].[Y+3].[Cu+2] GWHUBCMJWKDESZ-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000000126 substance Substances 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
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of yttrium oxide dispersion strengthened copper, which comprises the following steps: firstly, carrying out oxidation treatment on copper powder to obtain oxidized copper powder; secondly, carrying out two-step high-energy ball milling treatment on the oxidized copper powder and yttrium oxide, and then carrying out vacuum drying to obtain mixed powder; thirdly, carrying out thermal reduction treatment on the mixed powder to obtain composite powder; and fourthly, performing discharge plasma sintering on the composite powder to obtain the yttrium oxide dispersion strengthened copper. According to the invention, copper powder is oxidized to effectively reduce the plasticity of the copper powder, and then the copper powder and yttrium oxide are subjected to high-energy ball milling treatment in two steps, so that the oxidized copper powder is further refined, the yttrium oxide is more uniformly distributed in the mixed powder, the agglomeration of yttrium oxide reinforcements in the yttrium oxide dispersion strengthened copper is avoided, the content of yttrium oxide is effectively improved, the mechanical property of the yttrium oxide dispersion strengthened copper is further improved, and the method is simple and easy to realize.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite material preparation, and particularly relates to a preparation method of yttrium oxide dispersion strengthened copper.
Background
The dispersion strengthening copper-based composite material has the advantages that the nano-scale second phase particles with high thermodynamic stability, stable chemical properties and high strength are uniformly dispersed in the copper matrix, so that the strength of the matrix material is greatly strengthened, and the excellent conductivity of copper is kept as far as possible, therefore, the dispersion strengthening copper-based composite material has wide application in aerospace and electronic and electrical industries. Among the plurality of second phase particles, rare earth oxide particles such as yttrium oxide are considered to be the most suitable dispersion-strengthened phase. The yttrium oxide has high-temperature thermodynamic stability, good refrigeration efficiency and excellent creep resistance and fatigue resistance; more importantly, the yttrium oxide has a fluorite-like structure and is in a position matching relationship with the copper matrix under proper conditions, so that the cutting particles can be strengthened. However, although the strength of the material is improved by adding the dispersion strengthening phase, the particles of the reinforcement are easy to agglomerate along with the increase of the content of the reinforcement, and further the comprehensive performance of the material is influenced. The existing single ball milling process cannot realize the uniform dispersion of the reinforcement, and how to effectively reduce the agglomeration of the reinforcement is an urgent problem to be solved at present.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing yttrium oxide dispersion strengthened copper, aiming at the defects of the prior art. According to the method, copper powder is oxidized to effectively reduce the plasticity of the copper powder, and then the copper powder and yttrium oxide are subjected to high-energy ball milling treatment in two steps, so that the oxidized copper powder is further refined, the yttrium oxide is more uniformly distributed in mixed powder, uniform dispersion of the yttrium oxide is realized, agglomeration of an yttrium oxide reinforcement body in yttrium oxide dispersion strengthened copper is avoided, and the mechanical property of the yttrium oxide dispersion strengthened copper is further improved.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing yttrium oxide dispersion strengthened copper is characterized by comprising the following steps:
the method comprises the following steps of firstly, carrying out oxidation treatment on copper powder to generate an oxidation film on the surface of the copper powder to obtain oxidized copper powder;
step two, carrying out two-step high-energy ball milling treatment on the oxidized copper powder obtained in the step one and yttrium oxide, and then carrying out vacuum drying to obtain mixed powder;
step three, carrying out thermal reduction treatment on the mixed powder obtained in the step two to obtain composite powder;
and step four, performing discharge plasma sintering on the composite powder obtained in the step three to obtain the yttrium oxide dispersion strengthened copper.
According to the invention, copper powder is firstly subjected to oxidation treatment, an oxidation film containing nano oxide particles is generated on the surface of the copper powder, the plasticity of the copper powder is effectively reduced, and then the copper powder and yttrium oxide are subjected to high-energy ball milling treatment in two steps, the plasticity of the oxidized copper powder is reduced, and the oxidized copper powder is easy to deform through the high-energy ball milling treatment, so that the size of the oxidized copper powder is further refined, the yttrium oxide is more uniformly distributed in mixed powder, and meanwhile, the agglomeration of the yttrium oxide is reduced through the two-step high-energy ball milling treatment, and the purpose of uniformly dispersing the yttrium oxide is; and (3) reducing an oxide film containing nano oxide particles generated on the surface of the copper powder in the mixed powder to generate copper nano particles through subsequent thermal reduction treatment, realizing the nano-scale dispersion effect, thus obtaining composite powder with uniformly dispersed copper and yttrium oxide, and sintering and molding to obtain the yttrium oxide dispersion strengthened copper. In conclusion, the method of the invention realizes the uniform dispersion of yttrium oxide, avoids the agglomeration of yttrium oxide reinforcement in yttrium oxide dispersion strengthened copper, and improves the mechanical property of yttrium oxide dispersion strengthened copper.
The preparation method of the yttrium oxide dispersion strengthened copper is characterized in that the temperature of the oxidation treatment in the first step is 250-450 ℃. The preferable temperature is favorable for forming an oxide film containing nano oxide particles on the surface of the copper powder, and the oxidized copper powder is easy to disperse and is not easy to agglomerate.
The preparation method of the yttrium oxide dispersion strengthened copper is characterized in that the mass ratio of yttrium oxide in the second step to copper powder in the first step is 1: 200-5.92: 200. the preferred mass ratio ensures the addition of yttria and facilitates the dispersion of yttria.
The preparation method of the yttrium oxide dispersion strengthened copper is characterized in that the rotation speed adopted by the two-step high-energy ball milling treatment in the second step is 450 rpm. The optimized rotating speed is beneficial to further refining the oxidized copper powder, and simultaneously, the agglomeration of yttrium oxide is effectively reduced.
The preparation method of the yttrium oxide dispersion strengthened copper is characterized in that in the fourth step, the temperature of the spark plasma sintering is 850-1050 ℃, the pressure is 40-160 MPa, and the heat preservation time is 5-30 min. The composite material prepared by the optimized technological parameters has no obvious gap and high density.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, copper powder is oxidized, so that the plasticity of the copper powder is effectively reduced, and then the copper powder and yttrium oxide are subjected to high-energy ball milling treatment in two steps, so that the oxidized copper powder is further refined, yttrium oxide is more uniformly distributed in mixed powder, composite powder with copper and yttrium oxide uniformly dispersed is obtained through subsequent thermal reduction treatment and is sintered and molded, uniform dispersion of yttrium oxide is realized, agglomeration of yttrium oxide reinforcement in yttrium oxide dispersion strengthened copper is avoided, and the mechanical property of yttrium oxide dispersion strengthened copper is improved.
2. The invention adopts two-step high-energy ball milling treatment to reduce the agglomeration of the yttrium oxide and achieve the aim of uniformly dispersing the yttrium oxide.
3. The preparation process is simple and easy to realize.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is an SEM photograph of copper powder in example 1 of the present invention.
FIG. 2 EDS profile scan of the mixed powder prepared in example 1 of the invention.
FIG. 3 is an SEM image of a dispersion-strengthened yttrium oxide copper prepared in example 1 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, placing 200g of copper powder in an atmosphere, and carrying out oxidation treatment for 5 hours at the temperature of 250 ℃ to generate an oxide film on the surface of the copper powder to obtain oxidized copper powder;
step two, carrying out first-step high-energy ball milling treatment on the oxidized copper powder obtained in the step one, 2.96g of yttrium oxide and 60mL of ethanol for 6 hours under the condition that the rotating speed is 450rpm, then carrying out vacuum drying, adding 2.96g of yttrium oxide, carrying out second-step high-energy ball milling treatment for 6 hours under the condition that the rotating speed is 450rpm, and carrying out vacuum drying to obtain mixed powder;
step three, carrying out thermal reduction treatment on the mixed powder obtained in the step two at 400 ℃ for 4h to obtain composite powder; the reducing atmosphere adopted by the thermal reduction treatment is hydrogen-argon mixed gas with the hydrogen volume fraction of 8%;
step four, performing discharge plasma sintering on the composite powder obtained in the step three to obtain yttrium oxide dispersion strengthened copper; the temperature of the spark plasma sintering is 850 ℃, the pressure is 40MPa, and the heat preservation time is 10 min.
Fig. 1 is a SEM image of copper powder in this example, fig. 2 is an EDS scanning image of the mixed powder prepared in this example, and comparing fig. 1 and fig. 2, it can be seen that the copper powder is further refined and reduced in size after two-step high-energy ball milling treatment.
Fig. 3 is an SEM image of the yttria dispersion-strengthened copper prepared in this example, and it can be seen from fig. 3 that yttria is uniformly dispersed in the yttria dispersion-strengthened copper.
Example 2
The embodiment comprises the following steps:
step one, placing 200g of copper powder in an atmosphere, and carrying out oxidation treatment for 5 hours at the temperature of 300 ℃ to generate an oxide film on the surface of the copper powder to obtain oxidized copper powder;
step two, carrying out first-step high-energy ball milling treatment on the oxidized copper powder obtained in the step one, 0.5g of yttrium oxide and 60mL of ethanol for 6 hours under the condition that the rotating speed is 450rpm, then carrying out vacuum drying, then adding 0.5g of yttrium oxide, carrying out second-step high-energy ball milling treatment for 6 hours under the condition that the rotating speed is 450rpm, and carrying out vacuum drying to obtain mixed powder;
step three, carrying out thermal reduction treatment on the mixed powder obtained in the step two at 400 ℃ for 4h to obtain composite powder; the reducing atmosphere adopted by the thermal reduction treatment is hydrogen-argon mixed gas with the hydrogen volume fraction of 8%;
step four, performing discharge plasma sintering on the composite powder obtained in the step three to obtain yttrium oxide dispersion strengthened copper; the temperature of the spark plasma sintering is 900 ℃, the pressure is 100MPa, and the heat preservation time is 5 min.
Example 3
The embodiment comprises the following steps:
step one, placing 200g of copper powder in an atmosphere, and carrying out oxidation treatment for 5 hours at the temperature of 450 ℃ to generate an oxide film on the surface of the copper powder to obtain oxidized copper powder;
step two, carrying out first-step high-energy ball milling treatment on the oxidized copper powder obtained in the step one, 1.5g of yttrium oxide and 60mL of ethanol for 6 hours under the condition that the rotating speed is 450rpm, then carrying out vacuum drying, adding 1.5g of yttrium oxide, carrying out second-step high-energy ball milling treatment for 6 hours under the condition that the rotating speed is 450rpm, and carrying out vacuum drying to obtain mixed powder;
step three, carrying out thermal reduction treatment on the mixed powder obtained in the step two at 400 ℃ for 4h to obtain composite powder; the reducing atmosphere adopted by the thermal reduction treatment is hydrogen-argon mixed gas with the hydrogen volume fraction of 8%;
step four, performing discharge plasma sintering on the composite powder obtained in the step three to obtain yttrium oxide dispersion strengthened copper; the temperature of the discharge plasma sintering is 1050 ℃, the pressure is 160MPa, and the heat preservation time is 30 min.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A method for preparing yttrium oxide dispersion strengthened copper is characterized by comprising the following steps:
the method comprises the following steps of firstly, carrying out oxidation treatment on copper powder to generate an oxidation film on the surface of the copper powder to obtain oxidized copper powder;
step two, carrying out two-step high-energy ball milling treatment on the oxidized copper powder obtained in the step one and yttrium oxide, and then carrying out vacuum drying to obtain mixed powder;
step three, carrying out thermal reduction treatment on the mixed powder obtained in the step two to obtain composite powder;
and step four, performing discharge plasma sintering on the composite powder obtained in the step three to obtain the yttrium oxide dispersion strengthened copper.
2. The method of claim 1, wherein the temperature of the oxidation treatment in the first step is 250 ℃ to 450 ℃.
3. The method according to claim 1, wherein the mass ratio of the yttrium oxide in the second step to the copper powder in the first step is 1: 200-5.92: 200.
4. the method for preparing yttrium oxide dispersion-strengthened copper according to claim 1, wherein the rotation speed of the two-step high-energy ball milling treatment in the second step is 450 rpm.
5. The method for preparing yttrium oxide dispersion strengthened copper according to claim 1, wherein the temperature of the spark plasma sintering in the fourth step is 850-1050 ℃, the pressure is 40-160 MPa, and the holding time is 5-30 min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61149449A (en) * | 1984-12-24 | 1986-07-08 | Sumitomo Electric Ind Ltd | Composite material for lead frame for semiconductor device and its production |
| CN101250639A (en) * | 2008-03-27 | 2008-08-27 | 哈尔滨工业大学深圳研究生院 | Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof |
| CN106834791A (en) * | 2017-01-16 | 2017-06-13 | 江西理工大学 | A kind of rare earth oxide particles strengthen the preparation method of high-conductivity copper alloy |
| CN109136615A (en) * | 2018-10-30 | 2019-01-04 | 江西理工大学 | A kind of multistep ball milling prepares the preparation method of nano-ceramic particle dispersed and strengthened copper-based composite material with multistep vapour phase reduction |
| CN111408714A (en) * | 2020-04-29 | 2020-07-14 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material with dual-scale structure and in-situ growth |
| CN111451491A (en) * | 2020-04-29 | 2020-07-28 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material |
-
2020
- 2020-12-07 CN CN202011415658.0A patent/CN112391550A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61149449A (en) * | 1984-12-24 | 1986-07-08 | Sumitomo Electric Ind Ltd | Composite material for lead frame for semiconductor device and its production |
| CN101250639A (en) * | 2008-03-27 | 2008-08-27 | 哈尔滨工业大学深圳研究生院 | Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof |
| CN106834791A (en) * | 2017-01-16 | 2017-06-13 | 江西理工大学 | A kind of rare earth oxide particles strengthen the preparation method of high-conductivity copper alloy |
| CN109136615A (en) * | 2018-10-30 | 2019-01-04 | 江西理工大学 | A kind of multistep ball milling prepares the preparation method of nano-ceramic particle dispersed and strengthened copper-based composite material with multistep vapour phase reduction |
| CN111408714A (en) * | 2020-04-29 | 2020-07-14 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material with dual-scale structure and in-situ growth |
| CN111451491A (en) * | 2020-04-29 | 2020-07-28 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material |
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