CN116550975B - Preparation method of diamond/copper composite material - Google Patents
Preparation method of diamond/copper composite material Download PDFInfo
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- CN116550975B CN116550975B CN202310811655.6A CN202310811655A CN116550975B CN 116550975 B CN116550975 B CN 116550975B CN 202310811655 A CN202310811655 A CN 202310811655A CN 116550975 B CN116550975 B CN 116550975B
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- 239000010432 diamond Substances 0.000 title claims abstract description 164
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 164
- 239000010949 copper Substances 0.000 title claims abstract description 126
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 124
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 103
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000007747 plating Methods 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002060 nanoflake Substances 0.000 claims abstract description 20
- 238000007731 hot pressing Methods 0.000 claims abstract description 16
- 238000010146 3D printing Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 230000009471 action Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims description 5
- 229910039444 MoC Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910026551 ZrC Inorganic materials 0.000 claims description 4
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 18
- 238000003892 spreading Methods 0.000 abstract description 11
- 230000007480 spreading Effects 0.000 abstract description 11
- 230000000903 blocking effect Effects 0.000 abstract description 10
- 238000012856 packing Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 11
- 239000012467 final product Substances 0.000 description 7
- 238000004100 electronic packaging Methods 0.000 description 6
- 239000005022 packaging material Substances 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 101100456212 Arabidopsis thaliana MBD8 gene Proteins 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001374 Invar Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/006—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes with additional metal compounds being carbides
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Structural Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The application provides a preparation method of a diamond/copper composite material, which comprises the following steps: plating carbide on the surface of the diamond particles; carrying out chemical plating copper on the surfaces of the diamond particles plated with the carbide to obtain double-plating diamond powder; mixing the powder with micro-nano flake graphite powder to obtain mixed powder; carrying out high-temperature heat treatment on the mixed powder, infiltrating the diamond, shrinking the mixed powder into balls under the action of surface tension, and then cooling and solidifying along with a furnace; removing the micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, and preparing the high-heat-conductivity diamond/copper composite material through 3D printing or vacuum hot-pressing sintering. The copper-coated diamond spherical powder prepared by the method has the advantages of high sphericity, smooth surface, good fluidity, high loose packing density, difficult powder blocking phenomenon in the powder feeding or powder spreading process, high density of formed parts, uniform shrinkage of the formed parts in the sintering process, and high precision and thermal conductivity of the obtained diamond/copper composite material product.
Description
Technical Field
The application relates to the technical field of diamond/copper composite materials, in particular to a preparation method of a diamond/copper composite material.
Background
With the continuous development of microelectronic technology, the package integration level of semiconductors is higher and higher. The device is miniaturized, the power is larger and larger, and the requirement on the heat conducting property of the electronic packaging material is continuously improved. The thermal conductivity of the electronic packaging materials commonly used in the current integration can not meet the development requirements of integrated circuits and chip technologies far enough, so the development of the electronic packaging materials with higher thermal conductivity is urgent. The new generation of electronic packaging materials not only needs to have high heat conduction performance, but also needs to have thermal expansion performance matched with that of semiconductor materials.
The traditional heat conducting materials applied to the field of electronic packaging mainly comprise W/Cu, mo/Cu, invar alloy, kovar alloy and Al 2 O 3 AlN, silicon nitride and the like, which cannot meet application requirements due to low heat conductivity or high thermal expansion coefficient and the like, form a great threat to normal working efficiency and service life of the material, and particularly are urgent application requirements in the technical field of high technology which uses high-power Insulated Gate Bipolar Transistors (IGBT), vehicle-mounted high-power LED lamps, microwaves, electromagnetism, photoelectricity and the like as typical applications and the technical field of national defense which uses active phased array radars, high-energy solid lasers and the like as typical applications.
The diamond/copper composite material is called a fourth-generation electronic packaging material by virtue of the ultrahigh thermal conductivity and the adjustable thermal expansion coefficient, has the theoretical thermal conductivity as high as 1000W/(m.K), and has wide application prospect. However, the problems of poor interface bonding and wettability exist between copper and diamond, so that the composite material has low density and high interface thermal resistance, and the performance improvement and the thermal management application are seriously hindered. At present, titanium carbide, molybdenum carbide, zirconium carbide, chromium carbide and the like are plated on the surface of diamond, so that wettability and binding force with copper are improved, and interface thermal conductivity is improved.
In the prior art, as shown in fig. 4, the double-plated diamond powder prepared by adopting salt bath plating and chemical plating has the problems of rough surface, low sphericity, poor fluidity, low loose packing density and satellite powder, so that the powder feeding or spreading flow is not well controlled in the process of 3D printing or vacuum hot-pressing sintering, the powder blocking phenomenon is easy to occur, the density of a formed part is low, the shrinkage of the formed part is uneven in the sintering process, and the obtained diamond/copper composite material product has low precision and thermal conductivity (the thermal conductivity is generally about 550W/(m.K)).
Disclosure of Invention
Based on the above, the application aims to provide a preparation method of a diamond/copper composite material, which is used for solving the problems of low sphericity, poor fluidity and low loose packing density of copper-coated diamond powder in the prior art, which cause poor control of powder feeding or powder spreading flow in the process of 3D printing or vacuum hot-pressing sintering, easy occurrence of powder blocking phenomenon, void or defect of a final product, low density of a formed part, uneven shrinkage of the formed part in the sintering process, and low precision and thermal conductivity of the obtained diamond/copper composite material product.
The application provides a preparation method of a diamond/copper composite material, which comprises the following steps:
obtaining a plurality of diamond particles, and plating carbide on the surfaces of the diamond particles in a salt bath, wherein the carbide comprises molybdenum carbide, titanium carbide, tungsten carbide and zirconium carbide;
carrying out chemical plating copper treatment on the surfaces of the diamond particles plated with the carbide to prepare double-plating diamond powder;
uniformly mixing the double-coating diamond powder with a solid dispersing agent to obtain mixed powder, wherein the solid dispersing agent comprises micro-nano flake graphite powder;
carrying out high-temperature heat treatment on the mixed powder in a reducing atmosphere to enable copper to be molten and infiltrate into diamond, shrinking the mixed powder into balls under the action of surface tension, and then cooling and solidifying along with a furnace;
removing micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, and preparing the high-heat-conductivity diamond/copper composite material by adopting a 3D printing or vacuum hot-pressing sintering technology through the copper-coated diamond spherical powder.
According to the preparation method of the diamond/copper composite material, carbide and copper are plated on the surfaces of diamond particles in sequence to obtain double-plated diamond powder, the double-plated diamond powder and micro-nano flake graphite powder are uniformly mixed to obtain mixed powder, the mixed powder is subjected to high-temperature heat treatment in a reducing atmosphere to enable the copper to be molten and infiltrate into diamond, the diamond is contracted into balls under the action of surface tension, and then the diamond powder is cooled and solidified along with a furnace; the solid dispersing agent is removed to obtain copper-coated diamond spherical powder, the copper-coated diamond spherical powder has the advantages of smooth surface, high sphericity, good fluidity, high apparent density, and difficult powder blocking phenomenon in the powder feeding or powder spreading process, thereby ensuring the high heat conductivity and the product quality of the final product, and the density of the formed part is high, the shrinkage of the formed part is uniform in the sintering process, and the obtained diamond/copper composite material product has high precision and heat conductivity. The high-heat-conductivity diamond/copper composite material prepared by the copper-coated diamond spherical powder solves the technical problems that in the prior art, the sphericity of diamond powder and copper powder is low, the fluidity is poor, the loose packing density is low, the powder feeding or powder spreading flow is not well controlled in the 3D printing or vacuum hot-pressing sintering process, the powder blocking phenomenon easily occurs, the gap or defect of a final product is caused, the density of a formed part is low, the shrinkage of the formed part is uneven in the sintering process, and the precision and the heat conductivity of the obtained diamond/copper composite material product are low.
In addition, the preparation method of the diamond/copper composite material provided by the application can also have the following additional technical characteristics:
further, in the step of obtaining a plurality of diamond particles, plating carbide on the surface of the diamond particles in a salt bath:
the size of the selected diamond particles is 50um-300um, and the plating thickness of carbide is 200nm-1um.
Further, in the step of uniformly mixing the double-coated diamond powder with a solid dispersant to obtain a mixed powder:
the double-coating diamond powder and the micro-nano crystalline flake graphite powder are mixed by mechanical stirring, and the mixing mass ratio is 5:1-5, wherein the micro-nano crystalline flake graphite powder has a size of 200nm-1um.
Further, in the step of subjecting the mixed powder to a high-temperature heat treatment in a reducing atmosphere to melt copper and infiltrate diamond:
the high temperature heat treatment is heat treatment at a temperature 50-100 ℃ higher than the melting point of copper, and heat preservation is carried out for 5-10min, and the gas in the reducing atmosphere is one of hydrogen, hydrogen-argon mixed gas or carbon monoxide.
Further, in the step of removing the micro-nano flake graphite powder to obtain copper-coated diamond spherical powder:
soaking the obtained mixed powder with ethanol, and removing micro-nano flake graphite powder by ultrasonic cleaning to obtain copper-coated diamond spherical powder.
Further, removing micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, and preparing the high-heat-conductivity diamond/copper composite material by adopting a 3D printing or vacuum hot-pressing sintering technology through the copper-coated diamond spherical powder, wherein the preparation method comprises the following steps of:
when the copper-coated diamond spherical powder is prepared into the high-heat-conductivity diamond/copper composite material by adopting a vacuum hot-pressing sintering technology, the method comprises the following steps: directly filling copper-coated diamond spherical powder into a graphite mold to prepare the high-heat-conductivity diamond/copper composite material, wherein the pressure is 40MPa-80MPa, the temperature is 800-950 ℃, and the vacuum degree is 10 -2 Pa -10 -3 Pa, and preserving heat for 10min-50min.
Further, the prepared double-coating diamond powder has copper-containing volume fraction of 30% -60%.
Drawings
FIG. 1 is a scanning electron micrograph of a diamond feedstock used in an example of the present application;
FIG. 2 is a scanning electron microscope photograph of a molybdenum carbide-plated diamond obtained by salt bath plating according to the present application;
FIG. 3 is a scanning electron micrograph of copper-coated diamond spherical powder obtained by mixed heat treatment of copper-coated diamond powder and micro-nano flake graphite according to the present application;
fig. 4 is a scanning electron micrograph of copper-coated diamond powder prepared in the prior art.
The application will be further described in the following detailed description in conjunction with the above-described figures.
Detailed Description
In order that the application may be readily understood, a more complete description of the application will be rendered by reference to the appended drawings. Several embodiments of the application are presented in the figures. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In order to solve the problems that in the prior art, because the sphericity of the copper-coated diamond powder is not high, the fluidity is poor, the apparent density is low, the powder feeding or powder spreading flow is not well controlled in the 3D printing or vacuum hot-pressing sintering process, the powder blocking phenomenon is easy to occur, the final product is easy to generate gaps or defects, the density of a formed part is low, the shrinkage of the formed part is not uniform in the sintering process, and the precision and the heat conductivity of the obtained diamond/copper composite material product are low. The application provides a preparation method of a diamond/copper composite material, which is used for preparing a high-heat-conductivity diamond/copper composite material, wherein copper-coated diamond powder prepared by salt bath plating and chemical plating is mixed with micro-nano flake graphite powder, the mixture is subjected to heat treatment in a reducing atmosphere, copper melt is used for infiltrating the surface of the diamond, is not infiltrated with the micro-nano graphite powder at the same time, is contracted into balls, is finally cooled and solidified into balls to obtain copper-coated diamond spherical powder, and then the high-heat-conductivity diamond/copper composite material is prepared by adopting a 3D printing or vacuum hot-pressing sintering mode.
As shown in figures 1-3, the copper-coated diamond spherical powder manufactured by the method for manufacturing the diamond/copper composite material provided by the application has the advantages of high sphericity, controllable particle size distribution, narrow distribution, good fluidity, high apparent density and oxygen content below 100ppm, and the diamond/copper composite material with high heat conductivity is obtained by 3D printing or vacuum hot-pressing sintering technology, so that the diamond/copper composite material manufactured by the method has high product precision and high heat conductivity, and meanwhile, the process method is simple, the production efficiency is high, devices with complex shapes can be manufactured, and the method is a method for manufacturing the diamond/copper composite material with high heat conductivity in a large-scale manner.
The preparation method of the diamond/copper composite material provided by the application comprises the following steps of S11-S15:
s11, obtaining a plurality of diamond particles, and plating carbide on the surfaces of the diamond particles in a salt bath.
As a specific example, the carbide includes molybdenum carbide, titanium carbide, tungsten carbide, and zirconium carbide; specifically, carbide is plated on the surface of the diamond particles in a salt bath, so that the wettability and the binding property of diamond and a copper matrix are enhanced, the interface thermal resistance is reduced, and the thermal conductivity of the composite material is enhanced. Further, in this example, the diamond particle size was selected to be 50um to 300um, and the plating thickness of carbide was 200nm to 1um.
S12, carrying out chemical plating copper treatment on the surfaces of the diamond particles plated with the carbide to prepare double-plating diamond powder.
In this example, a double-coated diamond powder was prepared having a copper-containing volume fraction of 30% -60%.
And S13, uniformly mixing the double-coating diamond powder and the micro-nano flake graphite powder to obtain mixed powder.
In this embodiment, the mixing mode of the double-coated diamond powder and the micro-nano crystalline flake graphite powder is mechanical stirring mixing, and the mixing mass ratio is 5:1-5, wherein the micro-nano crystalline flake graphite powder has a size of 200nm-1um.
S14, carrying out high-temperature heat treatment on the mixed powder in a reducing atmosphere to enable copper to be molten and infiltrate into diamond, shrinking the mixed powder into balls under the action of surface tension, and then cooling and solidifying along with a furnace.
In the application, the mixed powder is subjected to high-temperature heat treatment in a reducing atmosphere, so that copper wrapped on the surface of diamond is melted and is not infiltrated with micro-nano flake graphite powder, and the mixed powder is contracted into balls under the action of surface tension and then cooled and solidified along with a furnace. By utilizing the characteristic that solid and liquid between copper and micro-nano crystalline flake graphite powder are not infiltrated, copper is melted and infiltrated into diamond, the diamond is contracted into balls under the action of surface tension, and then the balls are cooled and solidified along with a furnace, so that copper-coated diamond spherical powder is obtained. Specifically, the high-temperature heat treatment is carried out at a temperature 50-100 ℃ higher than the melting point of copper, and the temperature is kept for 5-10min, and the gas in the reducing atmosphere is hydrogen, hydrogen-argon mixture or carbon monoxide.
S15, removing the micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, and preparing the high-heat-conductivity diamond/copper composite material by adopting a 3D printing or vacuum hot-pressing sintering technology through the copper-coated diamond spherical powder.
Specifically, the obtained mixed powder is soaked in ethanol, and micro-nano flake graphite powder is removed through ultrasonic cleaning to obtain copper-coated diamond spherical powder. According to the application, the characteristics of high sphericity, smooth surface, good fluidity and high loose packing density of the copper-coated diamond spherical powder are utilized, and the powder blocking phenomenon is not easy to occur in the powder feeding or powder spreading process during 3D printing or vacuum hot-pressing sintering, so that the high heat conductivity and the product quality of the final product are ensured.
As a specific example, when the copper-coated diamond spherical powder is prepared into a high thermal conductivity diamond/copper composite material by using a vacuum hot-pressed sintering technology: directly filling copper-coated diamond spherical powder into a graphite mold to prepare the high-heat-conductivity diamond/copper composite material, wherein the pressure is 40MPa-80MPa, the temperature is 800-950 ℃, and the vacuum degree is 10 - 2 Pa-10 -3 Pa, and preserving heat for 10min-50min.
In order to facilitate an understanding of the application, several embodiments of the application will be presented below. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
The preparation method of the diamond/copper composite material in the embodiment comprises the following steps:
in the present embodiment, the MBD8 type diamond powder having an average size of about 100um is preferable as the raw material, and in this embodiment, the MBD8 type diamond powder having a size of 100um is preferably obtained by subjecting diamond particles to degreasing treatment with ethanol and acetone first, followed by 15% naoh solution and 30% hno solution, respectively 3 The solution is boiled to perform activation and coarsening treatment, and then is washed by deionized water and dried. Loading the pretreated diamond particles and molybdenum powder into a ball milling tank according to a molar ratio of 10:1, adding 2wt% alcohol, and ball milling and mixing for 2 hours at 200rpm, wherein the ball-to-ball ratio is 1:1; and (3) filling the mixed powder into an alumina crucible, and spreading mixed salt (NaCl: KCl molar ratio is 1:1) on the surface of the mixed powder, wherein the mass ratio of the mixed powder to the mixed salt is 1:2. And then placing the crucible into a vacuum tube furnace, performing reaction sintering for 15min at 1050 ℃, heating and cooling at a rate of 5 ℃/min, cooling to 300 ℃, taking out after natural cooling, ultrasonically cleaning with deionized water to dissolve and remove chloride, and drying. Preparing an electroless plating solution: cu (Cu) 2 SO 4 ·5H 2 O(15g/L),Na 2 EDTA·2H 2 O (30 g/L) and formaldehyde HCHO (37% 15 ml/L), preparing plating solution ph to be 12-13 by using NaOH (10 mol/L) solution, reacting diamond particles plated with a molybdenum carbide layer in the plating solution at 45 ℃ for 12 hours, and washing and drying to obtain double-plating diamond powder with a copper plating layer on the surface.
The double-coated diamond powder is then mixed with flake graphite powder of about 400nm in size, preferably 400nm in this example, in a mass ratio of 5:3, and the mixture is mechanically stirred.
Placing the mixed powder of the mixed double-coating diamond powder/flake graphite into an alumina crucible, placing the crucible into a heating zone of a annealing furnace, and vacuumizing to 6 multiplied by 10 -3 Pa, then introducing hydrogen of 0.02MPa, heating to 550 ℃, and preserving heat for 30min. Then the heating area of the annealing furnace is quickly heated to 1150 ℃ to lead the temperature to be higher than the melting point of copper, and after the heat preservation is carried out for 5 minutes, the annealing furnace is cooled along with the furnace to solidify into balls.
Soaking the obtained mixed powder in ethanol, and performing ultrasonic cleaning to obtain copper-coated diamond spherical powder. Fig. 3 is a scanning electron micrograph of the appearance of the obtained copper-coated diamond spherical powder, from which it can be obtained, and the copper-coated diamond spherical powder prepared by the preparation method of the present application has a smooth surface and a high sphericity, so that the copper-coated diamond spherical powder has good fluidity, is convenient for controlling the flow rate of powder feeding or powder spreading, and avoids the occurrence of the powder blocking phenomenon, and in this embodiment, the spherical particle size is 120um to 180um, and the oxygen content is 83ppm. Finally, the obtained copper-coated diamond spherical powder is filled into a graphite mold, and the vacuum hot-pressing sintering mode is adopted, the pressure is 70MPa, the temperature is 850 ℃, and the heat preservation is carried out for 20min. The diamond/copper composite material is obtained after cooling, and the thermal conductivity of the diamond/copper composite material is 723W/(m.K) measured by using a laser thermal conductivity meter.
In summary, according to the preparation method of the diamond/copper composite material in the above embodiment of the present application, carbide and copper are plated on the surface of diamond particles in order to obtain double-plated diamond powder, then the double-plated diamond powder is uniformly mixed with micro-nano flake graphite powder to obtain mixed powder, the mixed powder is subjected to high temperature heat treatment in a reducing atmosphere to melt and infiltrate copper into diamond, and is shrunk into balls under the action of surface tension, and then cooled and solidified along with a furnace, and the solid dispersing agent is removed to obtain copper-coated diamond spherical powder. The copper-coated diamond spherical powder has the advantages of smooth surface, high sphericity, good fluidity, high apparent density, difficult powder blocking phenomenon in the powder feeding or powder spreading process, high thermal conductivity and product quality of the final product, high density of the formed part, uniform shrinkage of the formed part in the sintering process, and high precision and thermal conductivity of the obtained diamond/copper composite material product. The high-heat-conductivity diamond/copper composite material prepared by the copper-coated diamond spherical powder solves the problems that in the prior art, the copper-coated diamond powder has rough surface, low sphericity, poor fluidity and low loose density, so that the powder feeding or powder spreading flow is not well controlled in the 3D printing or vacuum hot-pressing sintering process, the powder blocking phenomenon easily occurs, the final product has gaps or defects, the density of a formed part is low, the shrinkage of the formed part is uneven in the sintering process, and the obtained diamond/copper composite material product has low precision and heat conductivity.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (6)
1. A method of preparing a diamond/copper composite comprising:
obtaining a plurality of diamond particles, and plating carbide on the surfaces of the diamond particles in a salt bath, wherein the carbide comprises molybdenum carbide, titanium carbide, tungsten carbide and zirconium carbide;
carrying out chemical plating copper treatment on the surfaces of the diamond particles plated with the carbide to prepare double-plating diamond powder;
uniformly mixing the double-coating diamond powder with a solid dispersing agent to obtain mixed powder, wherein the solid dispersing agent comprises micro-nano flake graphite powder;
carrying out high-temperature heat treatment on the mixed powder in a reducing atmosphere to enable copper to be molten and infiltrate into diamond, shrinking the mixed powder into balls under the action of surface tension, and then cooling and solidifying along with a furnace;
removing micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, and preparing the high-heat-conductivity diamond/copper composite material by adopting a 3D printing or vacuum hot-pressing sintering technology through the copper-coated diamond spherical powder;
in the step of subjecting the mixed powder to a high-temperature heat treatment in a reducing atmosphere to melt copper and infiltrate diamond:
the high temperature heat treatment is heat treatment at a temperature 50-100 ℃ higher than the melting point of copper, and heat preservation is carried out for 5-10min, and the gas in the reducing atmosphere is one of hydrogen, hydrogen-argon mixed gas or carbon monoxide.
2. The method of preparing a diamond/copper composite according to claim 1, wherein in the step of obtaining a plurality of diamond particles and plating carbide on the surface of the diamond particles in a salt bath:
the size of the selected diamond particles is 50um-300um, and the plating thickness of carbide is 200nm-1um.
3. The method of producing a diamond/copper composite according to claim 1, wherein in the step of uniformly mixing the double-coated diamond powder with a solid dispersing agent to obtain a mixed powder:
the double-coating diamond powder and the micro-nano crystalline flake graphite powder are mixed by mechanical stirring, and the mixing mass ratio is 5:1-5, wherein the micro-nano crystalline flake graphite powder has a size of 200nm-1um.
4. The method of producing a diamond/copper composite material according to claim 1, wherein in the step of removing the micro-nano flake graphite powder to obtain copper-coated diamond spherical powder:
soaking the obtained mixed powder with ethanol, and removing micro-nano flake graphite powder by ultrasonic cleaning to obtain copper-coated diamond spherical powder.
5. The method of preparing a diamond/copper composite material according to claim 1, wherein the step of removing micro-nano flake graphite powder to obtain copper-coated diamond spherical powder, preparing the high thermal conductivity diamond/copper composite material by using 3D printing or vacuum hot press sintering technology through the copper-coated diamond spherical powder comprises:
when the copper-coated diamond spherical powder is prepared into the high-heat-conductivity diamond/copper composite material by adopting a vacuum hot-pressing sintering technology, the method comprises the following steps: directly filling copper-coated diamond spherical powder into a graphite mold to prepare the high-heat-conductivity diamond/copper composite material, wherein the pressure is 40MPa-80MPa, the temperature is 800-950 ℃, and the vacuum degree is 10 -2 Pa-10 -3 Pa, and preserving heat for 10min-50min.
6. The method for preparing diamond/copper composite material according to claim 1, wherein the prepared double-coated diamond powder has a copper-containing volume fraction of 30% -60%.
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