CN114713821B - 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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- CN114713821B CN114713821B CN202210033385.6A CN202210033385A CN114713821B CN 114713821 B CN114713821 B CN 114713821B CN 202210033385 A CN202210033385 A CN 202210033385A CN 114713821 B CN114713821 B CN 114713821B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 106
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004070 electrodeposition Methods 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 239000011258 core-shell material Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims description 38
- 238000009713 electroplating Methods 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000006185 dispersion Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 4
- 239000011162 core material Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000007747 plating 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
- 239000000306 component Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 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
- 238000004321 preservation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 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
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 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
Classifications
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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 processes: 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 graphene has the 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 has low cost and good arc ablation resistance.
Description
Technical Field
The invention belongs to the technical field of preparation of metal matrix composite materials, and relates to a preparation method of a Cu-W graphene-containing composite material.
Background
The vacuum switch electrical appliance 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 switch electrical appliance of a medium-high voltage power grid and an electrified railway. However, the absence of quenching gases places higher demands on the arc erosion resistance of the Cu-W contact material as a core component.
The addition of a third component, such as a carbide with a high melting point and a rare earth element with a low electron work function and oxides thereof, can diffusion strengthen the W skeleton strength and disperse the arc in the composite material. However, the addition of the third component can hinder 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. Graphene has excellent electric conduction, heat conduction 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 combination between the W skeleton strength and the electric conduction and heat conduction properties of the Cu-W composite, so that the exertion of the intrinsic excellent properties of the graphene is greatly limited.
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 strength of a W skeleton of the Cu-W composite material and the electric conduction and heat conduction properties.
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 and 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 liquid into the electrodeposition device;
step 1.2, uniformly dispersing graphene oxide in deionized water to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating liquid to obtain composite electroplating liquid;
and 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product with deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven to dry to obtain W@Cu & graphene core-shell powder.
In the step 1.1, the electroplating solution is obtained by uniformly mixing the CuSO4 with the concentration of 30-40 g/mL and the H2SO4 with the concentration of 70-90 mL 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 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.
The specific process of the step 2 is as follows:
step 2.1, performing cold press preforming on the W@Cu & graphene core-shell powder prepared in the step 1 to obtain a W@Cu & graphene green body;
and 2.2, sintering the W@Cu & graphene green body 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, equipment adopted by hot-press sintering is vacuum hot-press furnace or discharge plasma sintering equipment, and 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 of the Cu-W graphene-containing composite material has the beneficial effects that the graphene oxide in the preparation method of the Cu-W graphene-containing composite material adopts the reduced graphene oxide obtained by electrochemical reduction of the graphene oxide in the electrodeposition process, so that the production cost is greatly reduced. According to the preparation method, the distribution of graphene in the composite material can be regulated by regulating intermittent electrodeposition parameters, so that the tungsten skeleton strength is improved, and meanwhile, the conductivity of the material 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 and 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 metallic copper or stainless steel, an anode plate is placed parallel to the cathode plate, the anode plate is made of metallic elemental copper, and electroplating bath of the electrodeposition device is filled with electroplating solution;
passing the electroplating solution through CuSO 4 The concentration of (C) is 30-40 g/mL, H 2 SO 4 The concentration of (2) is 70-90 mL/L, and the mixture is uniformly mixed in deionized water;
step 1.2, uniformly dispersing graphene oxide in deionized water 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;
in the invention, graphene is reduced graphene oxide obtained by electrochemical reduction of graphene oxide in an 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 perform intermittent electrodeposition, cleaning a product with deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven to dry to obtain W@Cu & graphene core-shell powder, wherein the core material is W powder, and the shell layer is a composite layer of Cu and graphene;
the parameters of batch electrodeposition were: the current density is 1-7A/dm 2 The electrodeposition 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 comprises the following steps:
step 2.1, performing cold press preforming on the W@Cu & graphene core-shell powder prepared in the step 1, wherein the cold press pressure is 100-500 MPa, and obtaining a W@Cu & graphene green body;
step 2.2, sintering the W@Cu & graphene green body obtained in the step 2 for 100-120 min at 1300-1400 ℃ in an atmosphere tube furnace to obtain a Cu-W & graphene composite material;
or directly performing 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 adopted by hot-press sintering is a vacuum hot-press furnace or a 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 electrodeposition apparatus of the present application employs the deposition apparatus in CN 201710735384.5.
Example 1
Step 1, preparing W@Cu and graphene core-shell powder;
step 1.1, uniformly placing 50gW of powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of metallic copper, the anode plate is made of metallic elemental copper, and filling electroplating liquid into the electrodeposition device; the electroplating solution comprises the following components: cuSO 4 Is 30g/mL, H 2 SO 4 The concentration of (2) is 70mL/L, and the mixture is evenly mixed in deionized water to obtain the product;
step 1.2, placing 10mg of graphene oxide into 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into the electroplating liquid to obtain composite electroplating liquid;
step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product by deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven at 60 ℃ to dry for 2 hours to obtain W@Cu & graphene core-shell powder;
the parameters of batch electrodeposition were: the current density is 1A/dm2, the electrodeposition time is 45min, and the pulse width is 60s;
step 2.1, performing cold press 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 body;
step 2.2, placing the W@Cu & graphene green body obtained in the step 2.1 into an atmosphere tube furnace, and performing pressureless sintering at the temperature of 1400 ℃ for 120min to obtain a Cu-W & graphene composite material;
example 2
Step 1, preparing W@Cu and graphene core-shell powder;
step 1.1, uniformly placing 50gW of powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of metallic copper, the anode plate is made of metallic elemental copper, and filling electroplating liquid into the electrodeposition device; the electroplating solution comprises the following components: cuSO 4 Is 40g/mL, H 2 SO 4 The concentration of (2) is 70mL/L, and the mixture is evenly mixed in deionized water to obtain the product;
step 1.2, placing 50mg of graphene oxide into 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into the electroplating liquid to obtain composite electroplating liquid;
step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product by deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven at 60 ℃ to dry for 2 hours to obtain W@Cu & graphene core-shell powder;
the parameters of batch electrodeposition were: the current density is 5A/dm2, the electrodeposition time is 30min, and the pulse width is 120s;
step 2.1, carrying out cold press 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 body;
and 2.2, placing the W@Cu & graphene green body obtained in the step 2.1 into an atmosphere tube furnace, and performing 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, carrying out cold press 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 body;
and 2.2, placing the W@Cu & graphene green body obtained in the step 2.1 into an atmosphere tube furnace, and performing pressureless sintering at 1350 ℃ for 110min to obtain the Cu-W & graphene composite material.
Example 4
Step 1, preparing W@Cu and graphene core-shell powder;
step 1.1, uniformly placing 50gW of powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of stainless steel, the anode plate is made of elemental copper, and the electrodeposition device is filled with electroplating solution; the electroplating solution comprises the following components: cuSO 4 Is 35g/mL, H 2 SO 4 The concentration of (2) is 80mL/L, and the mixture is evenly mixed in deionized water;
step 1.2, placing 100mg of graphene oxide into 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into the electroplating liquid to obtain composite electroplating liquid;
step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product by deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven at 60 ℃ to dry for 2 hours to obtain W@Cu & graphene core-shell powder;
the parameters of batch electrodeposition were: the current density is 7A/dm2, the electrodeposition time is 10min, and the pulse width is 200s;
step 2, placing the W@Cu & graphene core-shell powder prepared in the step 1 into a vacuum hot pressing furnace, and obtaining a Cu-W & graphene composite material under the conditions that the sintering temperature is 1050 ℃, the heat preservation time is 30min and the pressure is 40 MPa;
example 5
Step 1, preparing W@Cu and graphene core-shell powder;
step 1.1, uniformly placing 50gW of powder on a cathode plate of an electrodeposition device, wherein the cathode plate is made of stainless steel, the anode plate is made of elemental copper, and the electrodeposition device is filled with electroplating solution; the electroplating solution comprises the following components: cuSO 4 Is 30g/mL, H 2 SO 4 The concentration of (2) is 90mL/L, and the mixture is uniformly mixed in deionized water;
step 1.2, placing 50mg of graphene oxide into 100ml of deionized water for uniform dispersion to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into the electroplating liquid to obtain composite electroplating liquid;
step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product by deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven at 60 ℃ to dry for 2 hours to obtain W@Cu & graphene core-shell powder;
the parameters of batch electrodeposition were: the current density is 5A/dm2, the electrodeposition time is 30min, and the pulse width is 120s;
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 under the pressure of 80MPa to obtain a Cu-W & graphene composite material;
example 6
The difference from example 5 is that: and 2, placing the W@Cu & graphene core-shell powder prepared in the step 1 into a discharge plasma sintering device, and obtaining the Cu-W & graphene composite material under the conditions that the temperature is 1300 ℃ and the heat preservation time is 100min and the pressure is 60 MPa.
Claims (3)
- The preparation method of the Cu-W graphene-containing composite material is characterized by comprising the following steps of:step 1, preparing W@Cu and graphene core-shell powder;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 liquid into the electrodeposition device;step 1.2, uniformly dispersing graphene oxide in deionized water to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating liquid to obtain composite electroplating liquid;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;step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product with deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven to dry to obtain W@Cu & graphene core-shell powder, wherein the core material is W powder, and the shell layer is a composite layer of Cu and graphene;in step 1.3, the parameters of 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;step 2, sintering the W@Cu & graphene core-shell powder prepared in the step 1 to obtain a Cu-W graphene-containing composite material;the specific process of the step 2 is as follows:step 2.1, performing cold press preforming on the W@Cu & graphene core-shell powder prepared in the step 1 to obtain a W@Cu & graphene green body;the cold pressing pressure is 100-500 MPa;step 2.2, sintering the W@Cu & graphene green body obtained in the step 2.1 to obtain a Cu-W graphene-containing composite material;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 preparation method of the Cu-W graphene-containing composite material is characterized by comprising the following steps of:step 1, preparing W@Cu and graphene core-shell powder;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 liquid into the electrodeposition device;step 1.2, uniformly dispersing graphene oxide in deionized water to obtain uniform dispersion liquid, and adding the uniform dispersion liquid into electroplating liquid to obtain composite electroplating liquid;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;step 1.3, conducting a pulse power supply to perform intermittent electrodeposition, cleaning a product with deionized water and alcohol after the electrodeposition is finished, and putting the product into a vacuum drying oven to dry to obtain W@Cu & graphene core-shell powder, wherein the core material is W powder, and the shell layer is a composite layer of Cu and graphene;in step 1.3, the parameters of 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;step 2, carrying out hot-pressing sintering on the W@Cu & graphene core-shell powder prepared in the step 1 to obtain a Cu-W graphene-containing composite material;in the step 2, equipment adopted by hot-press sintering is vacuum hot-press furnace or discharge plasma sintering equipment, and 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.
- 3. The method for producing a Cu-W graphene-containing composite material as claimed in claim 1 or 2, wherein in step 1.1, the plating solution is passed through CuSO 4 The concentration of (C) is 30-40 g/mL, H 2 SO 4 The concentration of (2) is 70-90 mL/L, and the mixture is uniformly mixed in deionized water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210033385.6A CN114713821B (en) | 2022-01-12 | 2022-01-12 | Preparation method of Cu-W graphene-containing composite material |
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| CN202210033385.6A CN114713821B (en) | 2022-01-12 | 2022-01-12 | Preparation method of Cu-W graphene-containing composite material |
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| CN114713821A CN114713821A (en) | 2022-07-08 |
| CN114713821B true CN114713821B (en) | 2024-03-12 |
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