CN114425622A - Powder metallurgy composite material and preparation method thereof - Google Patents
Powder metallurgy composite material and preparation method thereof Download PDFInfo
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- CN114425622A CN114425622A CN202210105309.1A CN202210105309A CN114425622A CN 114425622 A CN114425622 A CN 114425622A CN 202210105309 A CN202210105309 A CN 202210105309A CN 114425622 A CN114425622 A CN 114425622A
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- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000005245 sintering Methods 0.000 claims abstract description 70
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 64
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052802 copper Inorganic materials 0.000 claims abstract description 52
- 239000010949 copper Substances 0.000 claims abstract description 52
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 45
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000007731 hot pressing Methods 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000007740 vapor deposition Methods 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 19
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010301 surface-oxidation reaction Methods 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 11
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000000280 densification Methods 0.000 claims description 28
- 239000010410 layer Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 description 27
- 239000002270 dispersing agent Substances 0.000 description 9
- 230000017525 heat dissipation Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002470 thermal conductor Substances 0.000 description 1
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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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The application belongs to the technical field of powder metallurgy, and particularly discloses a powder metallurgy composite material and a preparation method thereof, wherein the preparation method comprises the steps of respectively carrying out low-energy ball milling on copper powder and aluminum powder to obtain smaller powder, and then respectively carrying out cold pressing to obtain a copper sheet blank and an aluminum sheet blank; sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove a surface oxidation film by ultrasonic treatment, and then sequentially cleaning with water, ethanol and acetone and drying in the air; transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box; after hot-pressing sintering is carried out in a sintering machine, the mixture is put into a vacuum furnace to be densified and sintered in an argon atmosphere. The method can effectively reduce the material cost of the copper material.
Description
Technical Field
The application belongs to the technical field of powder metallurgy, and particularly relates to a powder metallurgy composite material and a preparation method thereof.
Background
Copper and aluminum are widely applied to various electronic products as good thermal conductors, particularly heat dissipation substrates, and because the price of copper is relatively high, but the thermal conductivity of aluminum is relatively low, if the copper and the aluminum can be mixed according to a certain proportion, a composite material with low cost and good heat dissipation effect can be obtained.
Accordingly, further developments and improvements are still needed in the art.
Disclosure of Invention
In order to solve the above problems, a powder metallurgy composite material and a method for preparing the same are proposed. The application provides the following technical scheme:
the powder metallurgy composite material comprises an aluminum sheet and a copper sheet which are sequentially laminated and compounded, wherein single-layer graphene is attached to the surface of the copper sheet.
Further, the outermost layer of the composite material is a copper sheet.
A method of preparing a powder metallurgy composite material, comprising:
respectively carrying out low-energy ball milling on copper powder and aluminum powder to obtain smaller powder, and then respectively cold-pressing the powder into copper flake blanks and aluminum flake blanks;
sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove a surface oxidation film by ultrasonic treatment, and then sequentially cleaning with water, ethanol and acetone and drying in the air;
transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
after hot-pressing sintering is carried out in a sintering machine, the mixture is put into a vacuum furnace to be densified and sintered in an argon atmosphere.
Furthermore, the rotation speed of the low-energy ball mill is 100-150r/min, absolute ethyl alcohol is used as a dispersing agent, and the ball milling time is 4 hours.
Furthermore, the thickness of the sheet blank after cold pressing is 0.5-1 mm.
Further, when the surface oxide film is removed by ultrasonic, the thin sheet blank is respectively subjected to ultrasonic treatment in acetone, ethanol and water for 5min and ultrasonic treatment in dilute hydrochloric acid for 10 min.
Further, the gas flow ratio of methane, hydrogen and argon is 1:30:30-1:5:5, and the vapor deposition temperature is 1050 ℃.
Further, the flow rate of methane was 5sccm at the time of vapor deposition, and was increased to 30sccm after 10 min.
Further, the temperature of the hot-pressing sintering is 700-900 ℃, and the pressure is 500kgf/cm2And hot-pressing sintering time is 4 min.
Further, the densification sintering temperature is 1100 ℃, and the densification sintering time is 30 min.
Has the advantages that:
1. by compounding the copper sheet and the aluminum sheet, the heat dissipation efficiency is improved, and the material cost is reduced;
2. the graphene is vapor-deposited on the surface of the copper sheet, so that the oxidation of the surface of the copper sheet is prevented, and the heat conduction efficiency is improved;
3. the heat conduction efficiency is improved by removing an oxide layer of the sheet blank;
4. processing and synthesizing in an oxygen-free environment to avoid secondary formation of an oxide layer;
5. by controlling the gas flow ratio, the deposition of the thin graphene is realized, and the heat conduction loss of the copper sheet and the aluminum sheet crystal boundary is made up.
Drawings
FIG. 1 is a schematic flow chart of a powder metallurgy composite material and a preparation method thereof according to an embodiment of the present application;
FIG. 2 is a Raman spectrum of a vapor deposition product according to an embodiment of the present application;
fig. 3 shows different thermal conductivities for different sintering temperatures in the specific example of the present application.
Detailed Description
In order to make the technical solutions of the present application better understood, the following description of the technical solutions of the present application with reference to the drawings of the present application clearly and completely describes, and other similar embodiments obtained by a person of ordinary skill in the art without making creative efforts based on the embodiments of the present application shall fall within the protection scope of the present application. In addition, directional terms such as "upper", "lower", "left", "right", etc. in the following embodiments are directions with reference to the drawings only, and thus, the directional terms are used for illustration and not for limiting the present invention.
The powder metallurgy composite material comprises an aluminum sheet and a copper sheet which are sequentially laminated and compounded, wherein single-layer graphene is attached to the surface of the copper sheet.
Further, the outermost layer of the composite material is a copper sheet.
As shown in fig. 1, a method for preparing a powder metallurgy composite material comprises the following steps:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder to obtain smaller powder, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank;
s2, in an oxygen-free box, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid to remove a surface oxidation film by ultrasonic waves, and then sequentially cleaning by the water, the ethanol and the acetone and drying in the air;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box; after the graphene-copper sheet blank is corroded by a sulfuric acid solution, a transparent film floats above the solution, and the graphene is detected as graphene through Raman detection, as shown in FIG. 2.
And S4, performing hot-pressing sintering in a sintering machine, and then putting into a vacuum furnace to perform densification sintering in an argon atmosphere.
Further, the rotation speed of the low-energy ball milling is 100-150r/min, absolute ethyl alcohol is used as a dispersing agent, and the ball milling time is 4 hours.
Furthermore, the thickness of the sheet blank after cold pressing is 0.5-1 mm.
Further, when the surface oxide film is removed by ultrasonic, the thin sheet blank is respectively subjected to ultrasonic treatment in acetone, ethanol and water for 5min and ultrasonic treatment in dilute hydrochloric acid for 10 min.
Further, the gas flow ratio of methane, hydrogen and argon is 1:30:30-1:5:5, and the vapor deposition temperature is 1050 ℃.
Further, the flow rate of methane was 5sccm at the time of vapor deposition, and was increased to 30sccm after 10 min.
Further, the temperature of the hot-pressing sintering is 700-900 ℃, and the pressure is 500kgf/cm2And hot-pressing sintering time is 4 min.
Further, the densification sintering temperature is 1100 ℃, and the densification sintering time is 30 min.
The heat-conducting property of the heat-dissipating material prepared in the following examples was tested and analyzed by a laser flash point method using an LFA1000 thermal conductivity tester.
Example 1
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the hot-pressing sintering temperature is 700 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 50W/mK.
Example 2
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the hot-pressing sintering temperature is 750 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 54W/mK.
Example 3
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the hot-pressing sintering temperature is 800 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 57W/mK.
Example 4
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the copper powder and the aluminum powder into copper sheet blanks and aluminum sheet blanks after obtaining powder with smaller size, wherein the thickness of the cold-pressed sheet blanks is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the temperature of the hot-pressing sintering is 850 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 59W/mK.
Example 5
A method of making a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere at the temperature of 900 ℃ and under the pressure of 500 DEG Ckgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 58W/mK.
Example 6
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, wherein the flow rates of the methane, the hydrogen and the argon are respectively 5sccm, 150sccm and 150sccm, changing the flow rates into 30sccm, 150sccm and 150sccm after maintaining for 10min, performing vapor deposition at the temperature of 1080 ℃, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the hot-pressing sintering temperature is 950 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 57W/mK.
Comparative example
A method of preparing a powder metallurgy composite material, comprising:
s1, respectively carrying out low-energy ball milling on copper powder and aluminum powder at the rotation speed of 100-150r/min for 4h by using absolute ethyl alcohol as a dispersing agent, and then respectively cold-pressing the powder into a copper flake blank and an aluminum flake blank after obtaining powder with smaller size, wherein the thickness of the cold-pressed flake blank is 0.5-1 mm;
s2, sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove the surface oxidation film by ultrasonic treatment, wherein when the surface oxidation film is removed by ultrasonic treatment, the sheet blank is respectively subjected to ultrasonic treatment in the acetone, the ethanol and the water for 5min and in the dilute hydrochloric acid for 10min, and then is sequentially subjected to ultrasonic treatment in the water, the ethanol and the acetone for 30s, and is naturally dried;
s3, stacking the copper sheet blank and the aluminum sheet blank at intervals in an oxygen-free box, and then sealing, coating and discharging the copper sheet blank and the aluminum sheet blank;
s4, after hot-pressing sintering is carried out in a sintering machine, putting the sintered material into a vacuum furnace, and carrying out densification sintering in an argon atmosphere, wherein the temperature of the hot-pressing sintering is 850 ℃, and the pressure is 500kgf/cm2Hot-pressing sintering time is 4min, densification sintering temperature is 1100 ℃, and densification sintering time is 30 min. The thermal conductivity was 48W/mK.
As shown in fig. 3, which is a test result of the thermal conductivity, in a comparative example without adding graphene, since a copper grain boundary cannot be completely fused with an aluminum grain boundary, the thermal conductivity is low, and gaps of the copper grain boundary are filled by adding graphene, so that heat at the grain boundary is rapidly transferred out through the graphene.
It will be evident to those skilled in the art that the present application is not limited to the details of the foregoing illustrative embodiments, and that the present application may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
The above detailed description is only for the preferred embodiment of the present application, and the present application shall not be limited to the scope of the present application, and all equivalent changes and modifications shall be included in the scope of the present application.
Claims (10)
1. The powder metallurgy composite material is characterized by comprising an aluminum sheet and a copper sheet which are sequentially laminated and compounded, wherein single-layer graphene is attached to the surface of the copper sheet.
2. A powder metallurgical composite according to claim 1, wherein the outermost layer of the composite is a copper foil.
3. A method of preparing a powder metallurgical composite material according to claim 1, comprising:
respectively carrying out low-energy ball milling on copper powder and aluminum powder to obtain smaller powder, and then respectively cold-pressing the powder into copper flake blanks and aluminum flake blanks;
sequentially placing the sheet blank in acetone, ethanol, water and dilute hydrochloric acid in an oxygen-free box to remove a surface oxidation film by ultrasonic treatment, and then sequentially cleaning with water, ethanol and acetone and drying in the air;
transferring the copper sheet blank into a tubular furnace, introducing methane, hydrogen and argon to perform in-situ vapor deposition of graphene, transferring the deposited graphene-copper sheet blank into an oxygen-free box to be stacked with the aluminum sheet blank at intervals, and then sealing, coating and discharging the box;
after hot-pressing sintering is carried out in a sintering machine, the mixture is put into a vacuum furnace to be densified and sintered in an argon atmosphere.
4. The method as claimed in claim 3, wherein the rotation speed of the low-energy ball mill is 100-.
5. A method for preparing a powder metallurgical composite material according to claim 3, wherein the thickness of the cold-pressed laminar blank is 0.5-1 mm.
6. The method of claim 3, wherein the surface oxide film is removed by ultrasonic treatment, and the sheet material is subjected to ultrasonic treatment in acetone, ethanol and water for 5min and in dilute hydrochloric acid for 10 min.
7. The method for preparing the powder metallurgy composite material according to claim 3, wherein the gas flow ratio of methane, hydrogen and argon is 1:30:30-1:5:5, and the vapor deposition temperature is 1050 ℃.
8. The method as claimed in claim 7, wherein the flow rate of methane is increased to 30sccm after 10min after the vapor deposition, and the flow rate is 5 sccm.
9. The method as claimed in claim 3, wherein the hot-pressing sintering temperature is 700-900 deg.C and the pressure is 500kgf/cm2And hot-pressing sintering time is 4 min.
10. The method according to claim 3, wherein the densification sintering temperature is 1100 ℃ and the densification sintering time is 30 min.
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