CN114713821A - Preparation method of Cu-W graphene-containing composite material - Google Patents
Preparation method of Cu-W graphene-containing composite material Download PDFInfo
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- CN114713821A CN114713821A CN202210033385.6A CN202210033385A CN114713821A CN 114713821 A CN114713821 A CN 114713821A CN 202210033385 A CN202210033385 A CN 202210033385A CN 114713821 A CN114713821 A CN 114713821A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 102
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000004070 electrodeposition Methods 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 239000011258 core-shell material Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000009713 electroplating Methods 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000007731 hot pressing Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims 1
- 238000002490 spark plasma sintering Methods 0.000 claims 1
- 238000002679 ablation Methods 0.000 abstract description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000306 component Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 150000007524 organic acids Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000011156 metal matrix composite Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- 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
- B22F3/02—Compacting only
-
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a Cu-W graphene-containing composite material, which comprises the following specific steps: preparing W @ Cu & graphene core-shell powder by adopting an intermittent electrodeposition method, and then carrying out cold press molding and sintering on the W @ Cu & graphene core-shell powder to obtain a Cu-W & graphene composite material, or carrying out hot press sintering on the W @ Cu & graphene core-shell powder to obtain the Cu-W & graphene composite material. The method is expected to solve the problem that the addition of the graphene has a negative influence on the strength and the conductivity of the tungsten skeleton of the Cu-W composite material, and the method for preparing the composite material is low in cost and good in arc ablation resistance.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite preparation, and relates to a preparation method of a Cu-W graphene-containing composite.
Background
The vacuum switching device has the advantages of small volume, no pollution, good performance, no need of frequent maintenance, long service life and the like, and can be used as a leading switching device of medium and high voltage power grids and electrified railways. However, the absence of an arc-quenching gas places higher demands on the arc-erosion resistance of the Cu-W contact material as core component.
The addition of a third component, such as high-melting-point carbide and rare earth elements with low electronic work function and oxides thereof, can disperse and strengthen the W skeleton strength and disperse the electric arc in the composite material. However, the addition of the third component can block the movement of electrons and increase the scattering of phonons, reduce the conductivity of the material, prevent the heat from being transferred in time and accelerate the ablation rate of the composite material. The graphene has excellent electrical and thermal conductivity and mechanical properties, and is often used as a reinforcing phase to improve the comprehensive properties of the metal matrix composite, however, the addition of the graphene often causes the influence of the trade-off between the W framework strength and the electrical and thermal conductivity of the Cu-W composite, which greatly limits the exertion of the intrinsic excellent properties of the graphene.
Disclosure of Invention
The invention aims to provide a preparation method of a Cu-W graphene-containing composite material, which solves the problem that the addition of graphene affects the W framework strength and the electric and heat conducting properties of the Cu-W composite material.
The technical scheme adopted by the invention is that the preparation method of the Cu-W graphene-containing composite material is implemented according to the following steps:
step 1, preparing W @ Cu & graphene core-shell powder;
and 2, sintering the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain the Cu-W & graphene composite material.
The present invention is also characterized in that,
the specific process of the step 1 is as follows:
step 1.1, uniformly placing W powder on a cathode plate of an electrodeposition device, and filling electroplating solution into the electrodeposition device;
step 1.2, placing graphene oxide in deionized water to be uniformly dispersed to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating liquid to obtain composite electroplating liquid;
and step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning the product with deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven to obtain W @ Cu & graphene core-shell powder.
In the step 1.1, the electroplating solution is obtained by uniformly mixing CuSO4 with the concentration of 30-40 g/mL and H2SO4 with the concentration of 70-90 mL/L in deionized water.
In the step 1.2, the mass ratio of the W powder to the graphene oxide is 1: 0.02-0.2, and the mass volume ratio of the graphene oxide to the deionized water is 0.1-1 mg/ml.
In step 1.3, the parameters of the intermittent electrodeposition are as follows: the current density is 1-7A/dm 2, the electrodeposition time is 10-45 min, and the pulse width is 60-200 s.
The specific process of the step 2 is as follows:
step 2.1, carrying out cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain a W @ Cu & graphene green blank;
And 2.2, sintering the W @ Cu & graphene green blank obtained in the step 2.1 to obtain the Cu-W/graphene composite material.
In the step 2.1, the cold pressing pressure is 100-500 MPa; in the step 2.2, an atmosphere tube furnace is adopted for sintering, the sintering temperature is 1300-1400 ℃, and the sintering time is 100-120 min.
The specific process of the step 2 is as follows: and (3) carrying out hot-pressing sintering on the W @ Cu & graphene core-shell powder prepared in the step (1) to obtain the Cu-W & graphene composite material.
In the step 2, the equipment adopted by the hot-pressing sintering is a vacuum hot-pressing furnace or discharge plasma sintering equipment, and the sintering parameters are as follows: the sintering temperature is 900-1300 ℃, the sintering pressure is 40-80 MPa, and the sintering time is 10-100 min.
The preparation method has the beneficial effects that the reduced graphene oxide obtained by electrochemically reducing the graphene oxide in the electrodeposition process is adopted as the graphene oxide in the preparation method of the Cu-W graphene-containing composite material, so that the production cost is greatly reduced. According to the preparation method, the distribution of graphene in the composite material can be adjusted by adjusting the intermittent electrodeposition parameters, so that the conductivity of the material is improved while the strength of a tungsten framework is improved.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention provides a preparation method of a Cu-W graphene-containing composite material, which is implemented according to the following steps:
step 1, preparing W @ Cu & graphene core-shell powder;
the specific process is as follows:
step 1.1, uniformly placing W powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of metal copper or stainless steel, an anode plate is placed in parallel to the cathode plate, the anode plate is made of metal simple substance copper, and electroplating solution is filled in an electroplating bath of the electrodeposition device;
electroplating solution through CuSO4Has a concentration of 30-40 g/mL and H2SO4The concentration of the water-soluble organic acid is 70-90 mL/L, and the water-soluble organic acid is obtained by uniformly mixing the water-soluble organic acid and the organic acid in deionized water;
step 1.2, placing graphene oxide in deionized water to be uniformly dispersed to obtain uniform dispersion liquid, adding the uniform dispersion liquid into electroplating liquid, uniformly stirring to obtain composite electroplating liquid, and placing an anode plate into the composite electroplating liquid;
the graphene is reduced graphene oxide obtained by electrochemically reducing graphene oxide in the electrodeposition process;
the mass ratio of the W powder to the graphene oxide is 1: 0.02-0.2; the mass volume ratio of the graphene oxide to the deionized water is 0.1-1 mg/ml;
Step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning a product by using deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven to obtain W @ Cu & graphene core-shell powder, wherein the core material of the powder is W powder, and the shell layer is a composite layer of Cu and graphene;
the parameters of the batch electrodeposition are as follows: the current density is 1-7A/dm2The electro-deposition time is 10-45 min, and the pulse width is 60-200 s;
step 2, sintering the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain a Cu-W & graphene composite material;
the method specifically comprises the following steps:
step 2.1, performing cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1, wherein the cold pressing pressure is 100-500 MPa, and obtaining a W @ Cu & graphene green blank;
2.2, putting the W @ Cu & graphene green blank obtained in the step 2 into an atmosphere tube furnace at 1300-1400 ℃ for sintering for 100-120 min to obtain a Cu-W & graphene composite material;
or, directly carrying out hot-pressing sintering on the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain a Cu-W & graphene composite material;
wherein, the equipment that hot pressing sintering adopted is vacuum hot pressing stove or discharge plasma sintering equipment, and the sintering parameter is: the sintering temperature is 900-1300 ℃, the sintering pressure is 40-80 MPa, and the sintering time is 10-100 min.
The electrodeposition device of the present application employs the deposition device in CN 201710735384.5.
Example 1
Step 1, preparing W @ Cu & graphene core-shell powder;
step 1.1, uniformly placing 50gW powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of metal copper, and the anode plate is made of metal simple substance copper, and filling electroplating solution into the electrodeposition device; the electroplating solution is as follows: CuSO4Has a concentration of 30g/mL, H2SO4The concentration of (A) is 70mL/L, and the components are uniformly mixed in deionized water;
step 1.2, placing 10mg of graphene oxide in 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating solution to obtain composite electroplating solution;
step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning a product by using deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven at 60 ℃ for 2 hours to obtain W @ Cu & graphene core-shell powder;
the parameters of the batch electrodeposition are as follows: the current density is 1A/dm2, the electrodeposition time is 45min, and the pulse width is 60 s;
step 2.1, carrying out cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1 under the pressure of 100MPa to obtain a W @ Cu & graphene green blank;
2.2, placing the W @ Cu & graphene green blank obtained in the step 2.1 into an atmosphere tube furnace, and carrying out pressureless sintering at the temperature of 1400 ℃ for 120min to obtain a Cu-W & graphene composite material;
Example 2
Step 1, preparing W @ Cu & graphene core-shell powder;
step 1.1, uniformly placing 50gW powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of metal copper, and the anode plate is made of metal simple substance copper, and filling electroplating solution into the electrodeposition device; the electroplating solution is as follows: CuSO4Has a concentration of 40g/mL, H2SO4The concentration of (A) is 70mL/L, and the components are uniformly mixed in deionized water;
step 1.2, placing 50mg of graphene oxide in 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating solution to obtain composite electroplating solution;
step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning a product by using deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven at 60 ℃ for 2 hours to obtain W @ Cu & graphene core-shell powder;
the parameters of the batch electrodeposition are as follows: the current density is 5A/dm2, the electrodeposition time is 30min, and the pulse width is 120 s;
step 2.1, performing cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1 under the pressure of 500MPa to obtain a W @ Cu & graphene green blank;
and 2.2, placing the W @ Cu & graphene green blank obtained in the step 2.1 into an atmosphere tubular furnace, and carrying out pressureless sintering at the temperature of 1300 ℃ for 100min to obtain the Cu-W & graphene composite material.
Example 3
The difference from example 1 is that:
step 2.1, performing cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1 under the pressure of 300MPa to obtain a W @ Cu & graphene green blank;
and 2.2, placing the W @ Cu & graphene green blank obtained in the step 2.1 into an atmosphere tubular furnace, and carrying out pressureless sintering at the temperature of 1350 ℃ and the heat preservation time of 110min to obtain the Cu-W & graphene composite material.
Example 4
Step 1, preparing W @ Cu & graphene core-shell powder;
step 1.1, uniformly placing 50gW powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of stainless steel, and the anode plate is made of metal simple substance copper, and filling electroplating solution into the electrodeposition device; the electroplating solution is as follows: CuSO4Has a concentration of 35g/mL, H2SO4The concentration of (A) is 80mL/L, and the components are uniformly mixed in deionized water;
step 1.2, placing 100mg of graphene oxide in 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating solution to obtain composite electroplating solution;
step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning a product by using deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven at 60 ℃ for 2 hours to obtain W @ Cu & graphene core-shell powder;
The parameters of the batch electrodeposition are as follows: the current density is 7A/dm2, the electrodeposition time is 10min, and the pulse width is 200 s;
step 2, putting the W @ Cu & graphene core-shell powder prepared in the step 1 into a vacuum hot pressing furnace, and keeping the sintering temperature at 1050 ℃ for 30min and the pressure at 40MPa to obtain a Cu-W & graphene composite material;
example 5
Step 1, preparing W @ Cu & graphene core-shell powder;
step 1.1, uniformly placing 50gW powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of stainless steel, and the anode plate is made of metal simple substance copper, and filling electroplating solution into the electrodeposition device; the electroplating solution is as follows: CuSO4Has a concentration of 30g/mL, H2SO4The concentration of (A) is 90mL/L, and the components are uniformly mixed in deionized water;
step 1.2, placing 50mg of graphene oxide in 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating solution to obtain composite electroplating solution;
step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning a product by using deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven at 60 ℃ for 2 hours to obtain W @ Cu & graphene core-shell powder;
the parameters of the batch electrodeposition are as follows: the current density is 5A/dm2, the electrodeposition time is 30min, and the pulse width is 120 s;
Step 2, placing the W @ Cu & graphene core-shell powder prepared in the step 1 into a discharge plasma sintering device, and keeping the temperature at 900 ℃ for 10min and under the pressure of 80MPa to obtain a Cu-W & graphene composite material;
example 6
The differences from example 5 are: and 2, putting the W @ Cu & graphene core-shell powder prepared in the step 1 into a discharge plasma sintering device, and keeping the temperature at 1300 ℃ for 100min under the pressure of 60MPa to obtain the Cu-W & graphene composite material.
Claims (9)
- The preparation method of the Cu-W graphene-containing composite material is characterized by comprising the following steps:step 1, preparing W @ Cu & graphene core-shell powder;and 2, sintering the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain the Cu-W & graphene composite material.
- 2. The preparation method of the Cu-W graphene-containing composite material according to claim 1, wherein the specific process of the step 1 is as follows:step 1.1, uniformly placing W powder on a cathode plate of an electrodeposition device, and filling electroplating solution into the electrodeposition device;step 1.2, placing graphene oxide in deionized water to be uniformly dispersed to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating liquid to obtain composite electroplating liquid;And step 1.3, conducting a pulse power supply to carry out intermittent electrodeposition, cleaning the product with deionized water and alcohol after the electrodeposition is finished, and drying the product in a vacuum drying oven to obtain W @ Cu & graphene core-shell powder.
- 3. The method of claim 2, wherein in step 1.1, the plating solution is passed through CuSO4The concentration of (b) is 30-40 g/mL, H2SO4The concentration of (b) is 70-90 mL/L, and the components are uniformly mixed in deionized water to obtain the water-soluble glass.
- 4. The preparation method of the Cu-W graphene-containing composite material according to claim 2, wherein in the step 1.2, the mass ratio of W powder to graphene oxide is 1: 0.02-0.2, and the mass volume ratio of graphene oxide to deionized water is 0.1-1 mg/ml.
- 5. The method for preparing the Cu-W graphene-inclusive composite material according to claim 2, wherein in step 1.3, parameters of the batch electrodeposition are: the current density is 1-7A/dm 2, the electrodeposition time is 10-45 min, and the pulse width is 60-200 s.
- 6. The method for preparing the Cu-W graphene-containing composite material according to claim 1, wherein the specific process of the step 2 is as follows:step 2.1, carrying out cold pressing preforming on the W @ Cu & graphene core-shell powder prepared in the step 1 to obtain a W @ Cu & graphene green blank;And 2.2, sintering the W @ Cu & graphene green blank obtained in the step 2.1 to obtain the Cu-W & graphene composite material.
- 7. The preparation method of the Cu-W graphene-containing composite material according to claim 6, wherein in the step 2.1, the cold pressing pressure is 100-500 MPa; in the step 2.2, an atmosphere tube furnace is adopted for sintering, the sintering temperature is 1300-1400 ℃, and the sintering time is 100-120 min.
- 8. The preparation method of the Cu-W graphene-containing composite material according to claim 1, wherein the specific process of the step 2 is as follows: and (3) carrying out hot-pressing sintering on the W @ Cu & graphene core-shell powder prepared in the step (1) to obtain the Cu-W & graphene composite material.
- 9. The method for preparing the Cu-W graphene-containing composite material according to claim 8, wherein in the step 2, the equipment adopted by the hot-pressing sintering is a vacuum hot-pressing furnace or a spark plasma sintering equipment, and the sintering parameters are as follows: the sintering temperature is 900-1300 ℃, the sintering pressure is 40-80 MPa, and the sintering time is 10-100 min.
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