CN111850336B - Heat-conducting graphite composite material and preparation method thereof - Google Patents
Heat-conducting graphite composite material and preparation method thereof Download PDFInfo
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- 239000010439 graphite Substances 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 7
- 239000000020 Nitrocellulose Substances 0.000 claims description 7
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 7
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 7
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 7
- 229920001249 ethyl cellulose Polymers 0.000 claims description 7
- 229920000609 methyl cellulose Polymers 0.000 claims description 7
- 229920001220 nitrocellulos Polymers 0.000 claims description 7
- 238000002490 spark plasma sintering Methods 0.000 claims description 7
- 229940116411 terpineol Drugs 0.000 claims description 7
- 239000001761 ethyl methyl cellulose Substances 0.000 claims description 6
- 235000010944 ethyl methyl cellulose Nutrition 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 230000008030 elimination Effects 0.000 description 7
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- 238000000748 compression moulding Methods 0.000 description 6
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- 230000000704 physical effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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Abstract
The invention is applicable to the technical field of graphite composite materials, and provides a heat-conducting graphite composite material and a preparation method thereof, wherein the preparation method of the heat-conducting graphite composite material comprises the following steps: mixing flake graphite and aluminum powder, and then mixing the flake graphite and the aluminum powder with an interface impregnating compound to obtain mixed powder; mixing a binder and a solvent, and then mixing the mixture with the mixed powder to obtain slurry; printing the slurry on a substrate by a screen printing method, and drying to obtain a thick film; after the thick film is formed, organic matter removing treatment and cold isostatic pressing treatment are carried out to obtain a biscuit; and performing discharge plasma sintering on the biscuit to obtain the heat-conducting graphite composite material. The heat-conducting graphite composite material prepared by the preparation method has obvious high-orientation arrangement and high orientation degree, so that high heat-conducting performance can be realized on an xy plane.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a heat-conducting graphite composite material and a preparation method thereof.
Background
The rapid development of electronic equipment is promoted by the advancement of modern society science and technology, high-end electronic industrial devices are continuously developed towards high power density, miniaturization and function diversification, and the heat productivity and the heat flow are higher and higher, so that higher requirements are provided for the heat dissipation performance of the electronic equipment. At present, the heat dissipation structure adopted on the electronic device is generally made of metal materials such as aluminum, copper, silver and the like, and the metal materials have limited improvement degree of heat conductivity, heavy weight and large thermal expansion coefficient, so that the further wide use of the metal materials is greatly limited. The research and development of the novel composite material with high thermal conductivity, good mechanical property and light weight has very important significance for further miniaturization, light weight and high-efficiency operation of electronic equipment.
Today, where the properties of thermally conductive materials are continually challenging, researchers have attempted to replace traditional metallic materials with graphite materials. Graphite has low density, low expansion coefficient, excellent mechanical performance and very high thermal conductivity (2100 W.m) in xy plane-1·K-1) The heat conducting material has the most development potential in recent years. However, the graphite material has the disadvantages of low strength, poor toughness and easy pollution, and the simple substance is limited to be used for preparing the electronic packaging material. Aluminum is used as a common light metal heat dissipation material and has the advantages of high strength, corrosion resistance, low cost and the like. Therefore, after the advantages of the graphite and the aluminum are complemented, people find that the graphite-aluminum composite material as the electronic packaging heat conduction material has great research and application values.
The special layered molecular structure of the graphite material causes the atomic arrangement of the graphite material to have great difference in the direction parallel to the graphite sheet and the direction vertical to the graphite sheet, and the graphite material has obvious anisotropy. The structure ensures that the material has good thermal conductivity in the xy direction and can reach 900 W.m-1·K-1The conductivity in the z-axis direction is relatively poor, and is generally 20 to 30 W.m-1·K-1. The oriented arrangement of the flake graphite is beneficial to the heat conduction of heat along an x-y plane, and the urgent requirement of the heat management field on high heat conduction materials can be met as long as the size and preferred orientation of graphite microcrystals in the material are well controlled and the heat conductivity along the direction is improved. The graphite-aluminum composite material is a metal matrix composite material compounded by an aluminum matrix and graphite, previous researches have been focused on the mechanical property and the wear resistance of the graphite-aluminum composite material, and as people are continuously exploring good heat-conducting property in the direction of graphite layers, more and more scholars begin to research the thermal property of the composite material.
Currently, the orientation technology of flake graphite which is much studied is mainly the casting method. The national Ningbo material accumulates abundant experimental data and results in this respect, and aims to improve the thermal property of the graphite aluminum composite material to 500 W.m by a tape casting method-1·K-1(ii) a In the case of casting, the slurry is prepared during its operationThe drying process needs to be slowly dried in a solvent atmosphere because a casting film layer is thick (more than 0.1 mm), if slurry is not well controlled, the orientation degree of flake graphite crystal grains can be seriously influenced, the film layer is cracked, the thickness is not uniform and the like, and the technical process is very complicated.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a heat-conducting graphite composite material, and aims to solve the problems in the background art.
The embodiment of the invention is realized in such a way that the preparation method of the heat-conducting graphite composite material comprises the following steps:
mixing flake graphite and aluminum powder, and then mixing the flake graphite and the aluminum powder with an interface impregnating compound to obtain mixed powder;
mixing a binder and a solvent, and then mixing the mixture with the mixed powder to obtain slurry;
printing the slurry on a substrate by a screen printing method, and drying to obtain a thick film;
after the thick film is formed, organic matter removing treatment and cold isostatic pressing treatment are carried out to obtain a biscuit;
and performing discharge plasma sintering on the biscuit to obtain the heat-conducting graphite composite material.
As a preferable scheme of the embodiment of the invention, the mass ratio of the flake graphite, the aluminum powder and the interface sizing agent is (20-40): (60-80): 0.5-1).
As another preferable scheme of the embodiment of the present invention, the interface sizing agent is silicon powder.
As another preferable scheme of the embodiment of the invention, the mass ratio of the binder, the solvent and the mixed powder is 1 (15-20) to (10-15).
As another preferable mode of the embodiment of the present invention, the binder is at least one of ethyl cellulose, methyl cellulose, and nitrocellulose.
As another preferable mode of the embodiment of the present invention, the solvent is terpineol and/or ethylene glycol.
As another preferable scheme of the embodiment of the invention, in the step, the temperature of organic matter elimination treatment is 400-500 ℃; the temperature of the spark plasma sintering is 500-700 ℃, and the pressure is 30-50 MPa.
Another object of an embodiment of the present invention is to provide a heat conductive graphite composite material prepared by the above preparation method.
As another preferable solution of the embodiment of the present invention, the orientation degree of the heat conductive graphite composite material is not less than 90%.
The preparation method of the heat-conducting graphite composite material provided by the embodiment of the invention has the advantages of simple process, long service life of the prepared slurry, good stability and low cost, and can realize the industrial operation of a production line. The preparation method can control the thickness of the material film layer within a few microns, and the flake graphite elements in a single film layer can be well oriented under the action of the shearing force of the printing plate, so that the prepared heat-conducting graphite composite material has obvious high-orientation arrangement and high orientation degree, and can realize high heat-conducting performance on an xy plane.
Drawings
Fig. 1 is an XRD chart of the thermally conductive graphite composite material prepared in example 1 of the present invention.
Fig. 2 is an SEM image of the thermally conductive graphite composite material prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; mixing 300g of flake graphite and 700g of aluminum powder, and then mixing with 8g of interface wetting agent to obtain mixed powder; wherein, the flake graphite can pass through a 100-mesh sieve, namely the granularity can be controlled between 20 and 150 microns, the distribution is wide, and the density of the oriented layer is favorably improved.
S2, taking ethyl cellulose as a binder and terpineol as a solvent; heating, stirring and mixing 10g of binder and 180g of solvent to form a transparent solution, mixing with 120g of the mixed powder, and performing ball milling to obtain slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 95 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.25mm, wherein the thick film can be placed in the oven at 95 ℃ for drying for 18 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a 500-DEG C heat treatment furnace for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, placing the biscuit at the temperature of 600 ℃ and the sintering pressure of 40MPa for spark plasma sintering to obtain the heat-conducting graphite composite material.
Example 2
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; 200g of flake graphite and 800g of aluminum powder are mixed, and then mixed with 5g of interface wetting agent to obtain mixed powder.
S2, taking a mixture of ethyl cellulose, methyl cellulose and nitrocellulose in equal mass ratio as a binder, and taking a mixture of terpineol and glycol in equal volume ratio as a solvent; after 10g of a binder and 150g of a solvent were heated, stirred and mixed to form a transparent solution, the transparent solution was mixed with 100g of the above-mentioned mixed powder to obtain a slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 90 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.2mm, wherein the thick film can be placed in the oven at 90 ℃ for drying for 15 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a heat treatment furnace at 400 ℃ for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, placing the biscuit at the temperature of 500 ℃ and the sintering pressure of 30MPa for spark plasma sintering to obtain the heat-conducting graphite composite material.
Example 3
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; mixing 400g of flake graphite and 600g of aluminum powder, and then mixing with 10g of interface wetting agent to obtain mixed powder; wherein, the flake graphite can pass through a 100-mesh sieve, namely the granularity can be controlled between 20 and 150 microns, the distribution is wide, and the density of the oriented layer is favorably improved.
S2, taking a mixture of methylcellulose and nitrocellulose in equal mass ratio as a binder, and taking a mixture of ethylene glycol in equal volume ratio as a solvent; after 10g of the binder and 200g of the solvent were heated, stirred and mixed to form a transparent solution, the transparent solution was mixed with 150g of the above mixed powder, and ball-milled to obtain a slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 100 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.3mm, wherein the thick film can be placed in the oven at 100 ℃ for drying for 20 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a heat treatment furnace at 450 ℃ for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, placing the biscuit at the temperature of 700 ℃ and the sintering pressure of 50MPa for spark plasma sintering to obtain the heat-conducting graphite composite material.
Example 4
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; mixing 250g of flake graphite and 750g of aluminum powder, and then mixing with 6g of interface wetting agent to obtain mixed powder; wherein, the flake graphite can pass through a 100-mesh sieve, namely the granularity can be controlled between 20 and 150 microns, the distribution is wide, and the density of the oriented layer is favorably improved.
S2, taking a mixture of ethyl cellulose, methyl cellulose and nitrocellulose in equal mass ratio as a binder, and taking a mixture of terpineol and glycol in equal volume ratio as a solvent; after 10g of a binder and 160g of a solvent were heated, stirred and mixed to form a transparent solution, the transparent solution was mixed with 140g of the above mixed powder, and ball-milled to obtain a slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 90 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.2mm, wherein the thick film can be placed in the oven at 100 ℃ for drying for 17 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a heat treatment furnace at the temperature of 420 ℃ for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, placing the biscuit at the temperature of 550 ℃ and the sintering pressure of 35MPa for spark plasma sintering to obtain the heat-conducting graphite composite material.
Example 5
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; 350g of flake graphite and 650g of aluminum powder are mixed, and then mixed with 7g of interface wetting agent to obtain mixed powder; wherein, the flake graphite can pass through a 100-mesh sieve, namely the granularity can be controlled between 20 and 150 microns, the distribution is wide, and the density of the oriented layer is favorably improved.
S2, taking a mixture of ethyl cellulose, methyl cellulose and nitrocellulose in equal mass ratio as a binder, and taking a mixture of terpineol and glycol in equal volume ratio as a solvent; heating, stirring and mixing 10g of binder and 180g of solvent to form a transparent solution, mixing with 120g of the mixed powder, and performing ball milling to obtain slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 100 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.3mm, wherein the thick film can be placed in the oven at 90 ℃ for drying for 18 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a 480 ℃ heat treatment furnace for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, placing the biscuit at the temperature of 650 ℃ and the sintering pressure of 45MPa for spark plasma sintering to obtain the heat-conducting graphite composite material.
Example 6
The embodiment provides a preparation method of a heat-conducting graphite composite material, which comprises the following steps:
s1, taking flake graphite as an orientation element, aluminum powder as a matrix and silicon powder as an interface impregnating compound; mixing 280g of flake graphite and 720g of aluminum powder, and then mixing with 9g of interface wetting agent to obtain mixed powder; wherein, the flake graphite can pass through a 100-mesh sieve, namely the granularity can be controlled between 20 and 150 microns, the distribution is wide, and the density of the oriented layer is favorably improved.
S2, taking a mixture of ethyl cellulose, methyl cellulose and nitrocellulose in equal mass ratio as a binder, and taking a mixture of terpineol and glycol in equal volume ratio as a solvent; after 10g of the binder and 180g of the solvent were heated, stirred and mixed to form a transparent solution, the transparent solution was mixed with 140g of the above mixed powder, and ball-milled to obtain a slurry.
S3, printing the paste to a substrate through a screen printing method, then placing the substrate in an oven at 98 ℃ for drying treatment, and repeating the steps for multiple times to obtain a thick film with the thickness of 0.25mm, wherein the thick film can be placed in the oven at 90 ℃ for drying for 16 hours for later use.
And S4, cutting the thick film into thick film sheets with required size, taking the thick film sheets from the substrate, laminating the thick film sheets in a mould for compression molding, placing the thick film sheets in a heat treatment furnace at 450 ℃ for organic matter elimination treatment, and carrying out cold isostatic pressing treatment to obtain a biscuit.
And S5, performing discharge plasma sintering on the biscuit at the temperature of 620 ℃ and the sintering pressure of 40MPa to obtain the heat-conducting graphite composite material.
Experimental example:
the thermally conductive graphite composite material prepared in example 1 was subjected to an X-ray diffraction (XRD) test, and the XRD pattern obtained therefrom was as shown in fig. 1.
The thermally conductive graphite composite material obtained in example 1 was observed by a Scanning Electron Microscope (SEM), and the SEM image obtained is shown in fig. 2.
As can be seen from the attached drawings 1-2, the heat-conducting graphite composite material prepared by the embodiment of the invention has obvious high-orientation arrangement, the orientation degree of the heat-conducting graphite composite material reaches more than 90%, and the high heat-conducting performance is preliminarily realized on the xy surface of the heat-conducting graphite composite material.
In addition, the physical property test data of the heat-conducting graphite composite material prepared in embodiment 1 of the present invention are respectively as follows: the heat conductivity in the xy direction reaches 420W/mK, which is close to the heat conductivity of 450W/mK by adopting the traditional casting method, the thermal expansion coefficient is about 9ppm/K, and the density is 2.52g/cm3。
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. The preparation method of the heat-conducting graphite composite material is characterized by comprising the following steps of:
mixing flake graphite and aluminum powder, and then mixing the flake graphite and the aluminum powder with an interface impregnating compound to obtain mixed powder;
mixing a binder and a solvent, and then mixing the mixture with the mixed powder to obtain slurry;
printing the slurry on a substrate by a screen printing method, and drying to obtain a thick film;
after the thick film is formed, organic matter removing treatment and cold isostatic pressing treatment are carried out to obtain a biscuit;
performing discharge plasma sintering on the biscuit to obtain the heat-conducting graphite composite material;
wherein the mass ratio of the flake graphite to the aluminum powder to the interface sizing agent is (20-40) to (60-80) to (0.5-1); the interface impregnating compound is silicon powder; in the step, the temperature for removing the organic matters is 400-500 ℃; the temperature of the spark plasma sintering is 500-700 ℃, and the pressure is 30-50 MPa.
2. The method for preparing the heat-conducting graphite composite material as claimed in claim 1, wherein the mass ratio of the binder, the solvent and the mixed powder is 1 (15-20) to (10-15).
3. The method of claim 1 or 2, wherein the binder is at least one of ethyl cellulose, methyl cellulose and nitrocellulose.
4. The method of claim 1 or 2, wherein the solvent is terpineol and/or ethylene glycol.
5. A heat-conducting graphite composite material prepared by the preparation method of any one of claims 1 to 4.
6. A thermally conductive graphite composite material according to claim 5, wherein the degree of orientation of the thermally conductive graphite composite material is not less than 90%.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004035910A (en) * | 2002-06-28 | 2004-02-05 | Chuo Motor Wheel Co Ltd | Method for manufacturing aluminum composite |
CN103911565A (en) * | 2014-04-23 | 2014-07-09 | 北京科技大学 | Preparation method of high-thermal-conductivity graphite whisker-oriented and reinforced metal-based composite material |
CN108359825A (en) * | 2018-02-11 | 2018-08-03 | 太原理工大学 | A kind of preparation method of ceramics-graphene enhancing Cu-base composites |
CN108893636A (en) * | 2018-06-27 | 2018-11-27 | 北京科技大学 | A kind of preparation method of high thermal conductivity isotropic graphite ball reinforced aluminum matrix composites |
CN110079708A (en) * | 2019-06-20 | 2019-08-02 | 合肥工业大学 | A kind of method for preparing powder metallurgy of nano graphite flakes/Al alloy-base composite material |
-
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004035910A (en) * | 2002-06-28 | 2004-02-05 | Chuo Motor Wheel Co Ltd | Method for manufacturing aluminum composite |
CN103911565A (en) * | 2014-04-23 | 2014-07-09 | 北京科技大学 | Preparation method of high-thermal-conductivity graphite whisker-oriented and reinforced metal-based composite material |
CN108359825A (en) * | 2018-02-11 | 2018-08-03 | 太原理工大学 | A kind of preparation method of ceramics-graphene enhancing Cu-base composites |
CN108893636A (en) * | 2018-06-27 | 2018-11-27 | 北京科技大学 | A kind of preparation method of high thermal conductivity isotropic graphite ball reinforced aluminum matrix composites |
CN110079708A (en) * | 2019-06-20 | 2019-08-02 | 合肥工业大学 | A kind of method for preparing powder metallurgy of nano graphite flakes/Al alloy-base composite material |
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