CN114957897B - High-performance graphene film and preparation method thereof - Google Patents
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- C01B32/914—Carbides of single elements
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Abstract
The invention belongs to the technical field of heat conduction materials, and particularly relates to a high-performance graphene film and a preparation method thereof. The product developed by the invention comprises graphene particles; the graphene particles comprise layered graphene layers and spherical graphitized carbon microspheres embedded among the graphene layers; and, the spherical graphitized carbon microsphere is a hollow structure. In addition, the graphene particles also comprise carbon fibers, wherein the D50 of the graphene particles is 100-600 μm; the length distribution range of the carbon fiber is 200-300 mu m; the aspect ratio of the carbon fiber is 20:1-40:1; in addition, in the spherical graphitized carbon microsphere, silicon carbide is included. When a product is prepared, graphene oxide is dispersed in water, organic resin emulsion with the solid content of 30-50% is added, and after uniform ultrasonic dispersion, suction filtration and drying are carried out to obtain a precursor; and (3) carrying out high-temperature graphitization treatment on the precursor to obtain graphene particles, uniformly dispersing the graphene particles and the water-based acrylate emulsion, and then carrying out screen printing to form a film, thus obtaining the product.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials. And more particularly, to a high-performance graphene film and a method for preparing the same.
Background
The increase in power of the LED device results in an increase in junction temperature and a significant decrease in reliability and lifetime of the LED device. The graphite film with the thermal conductivity of only 300W/(m.K) used at present is difficult to meet the requirement of a high-power device on heat dissipation, so that the search for a heat dissipation material with high thermal conductivity becomes the key for the development of the field of microelectronics.
Graphene is a two-dimensional honeycomb lattice structure carbon material formed by stacking single-layer carbon atoms through sp2 hybridization, and is considered to be a heat-conducting thin film material with great development prospect due to excellent mechanical properties and thermal properties, particularly excellent heat-conducting property. The thermal conductivity of the suspended single-layer graphene at room temperature, which is reported at present, reaches 5300W/(m.K), which is far higher than that of graphite (about 2000W/(m.K)).
Although graphene is a heat dissipation material with a good application prospect, single-layer graphene cannot be directly used for lateral heat dissipation. Graphene Oxide (GO) is a precursor of graphene, and has good dispersibility in water, so that a graphene material can be easily prepared by performing thermal reduction treatment on a graphene oxide aqueous solution. However, GO contains a large number of oxygen-containing functional groups, which easily damages the structure and crystal integrity of graphene, and seriously affects the thermal conductivity of graphene.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect and the defect that the heat-conducting property of the existing graphene cannot be further improved when the graphene is used as a main functional additive of a heat-conducting film, and provides a high-performance graphene film and a preparation method thereof.
The invention aims to provide a high-performance graphene film.
The invention also aims to provide a preparation method of the high-performance graphene film.
The above purpose of the invention is realized by the following technical scheme:
a high performance graphene film comprising graphene particles; the graphene particles comprise layered graphene layers and spherical graphitized carbon microspheres embedded among the graphene layers;
and, the spherical graphitized carbon microsphere is a hollow structure.
Further, the graphene material also comprises carbon fibers, and the mass ratio of the carbon fibers to the graphene particles is 1:10-1:15.
further, the D50 of the graphene particles is 100-600 μm; the length distribution range of the carbon fiber is 200-300 mu m; the aspect ratio of the carbon fiber is 20:1-40:1.
further, the spherical graphitized carbon microsphere comprises silicon carbide.
Further, the coating also comprises a matrix resin, wherein the matrix resin is water-based acrylate.
A preparation method of a high-performance graphene film comprises the following specific preparation steps:
preparing graphene particles:
dispersing graphene oxide in water, adding an organic resin emulsion with the solid content of 30-50%, performing ultrasonic dispersion uniformly, performing suction filtration, and drying to obtain a precursor;
carrying out high-temperature graphitization treatment on the precursor to obtain graphene particles;
and (3) uniformly dispersing the graphene particles and the water-based acrylate emulsion, and then screen-printing to form a film, thus obtaining the product.
Further, the organic resin emulsion is selected from any one of styrene-acrylic emulsion, pure acrylic emulsion and silicone acrylic emulsion.
Further, the organic resin emulsion is selected from silicone-acrylic emulsion.
Further, the high-temperature graphitization treatment comprises: firstly, the precursor is subjected to heat preservation treatment for 2-3h at 1300-1400 ℃ under the protection of inert gas, then the temperature is raised to 2200-2400 ℃, and high-temperature graphitization treatment is carried out for 4-6h.
Further, the screen printing film formation includes:
fixing polyimide film as base film, silk screen printing on the surface, vacuum drying at 200 deg.C for 5-10min, and discharging.
The invention has the following beneficial effects:
(1) According to the technical scheme, in the preparation process of the graphene film, graphene oxide is dispersed to form a monolithic layer structure, then organic resin emulsion is added, spherical emulsion particles in the emulsion are adsorbed with oxygen-containing functional groups in a conjugated region and an edge region of the graphene oxide under the action of ultrasonic dispersion, in addition, in a matched suction filtration mode, the dispersed monolithic layer structure is stacked again, in the stacking process, the adsorbed spherical emulsion particles are fixed between the layers of the spherical emulsion particles, in the high-temperature graphitization process, firstly, the spherical emulsion particles deposited inside are gradually carbonized to form a hollow spherical carbon skeleton under the high-temperature condition of about 1300-1400 ℃, and then the temperature is continuously increased to a higher temperature to graphitize part of carbon, and the graphitized spherical carbon microspheres after graphitization are used as connecting sites between graphene layers, so that on one hand, the structure of a product can be effectively fixed, the layer spacing of the graphene cannot be obviously changed due to the change of the temperature in the use process of the product, and the heat conductivity and the consistency of the product can be effectively controlled; on the other hand, the existence of the spherical hollow graphitized carbon microspheres can be used as a good medium for heat transfer between layers, particularly a hollow spherical structure, heat can be rapidly transferred at the contact points of the spheres and the graphene sheet layers in all directions on the surfaces of the spheres, and the efficiency and the uniformity in the heat transfer process between layers are effectively improved;
(2) Further, by controlling the temperature of the graphitization process, the graphitized carbon microspheres between layers thereof are not completely graphitized, because the substantially amorphous carbon needs to be completely graphitized at a high temperature close to about 3000 ℃, and in the graphitizing temperature range controlled by the invention, part of the carbon still exists in an amorphous form, because excessive graphitization can further improve the structural stability of the graphitized microspheres, but the transfer efficiency and uniformity of the spheres formed by the regular arrangement of the graphitized carbon spheres are reduced when heat is transferred on the surfaces of the spheres, mainly because of the directionally arranged crystals, the heat conduction along the arrangement direction and the heat conduction coefficient perpendicular to the arrangement direction have a significant difference;
(3) Furthermore, in the preparation process of the precursor, preferably selecting silicone-acrylic emulsion, and before graphitization, carrying out treatment at 1300-1400 ℃, in the process, firstly, a carbonization process of organic matters is carried out, and then, si elements in the silicone-acrylic emulsion easily form Si-C with higher bond energy with C elements, so that the spherical structure of the silicone-acrylic emulsion is effectively stabilized, the structure is prevented from collapsing in the subsequent graphitization process, and the sphericity of the silicone-acrylic emulsion is effectively maintained, so that heat can be rapidly transferred on the contact points of the spherical body and the graphene sheet layer on the surface of the spherical body in each direction in the heat transfer process of the product, and the efficiency and uniformity in the heat transfer process between layers are effectively improved;
(4) In addition, a small amount of carbon fibers are introduced into the system, and in the film forming process, the fibrous structure of the carbon fibers and the lamellar structure of the graphene can form a continuous heat transfer three-dimensional network structure which is filled with each other, so that the temperature uniformity and the rapid transfer of the surface of the film layer are facilitated.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Preparing graphene particles:
mixing graphene oxide with D50 of 100 mu m and deionized water according to a mass ratio of 1:5, performing ultrasonic dispersion for 2 hours at the temperature of 45 ℃ and the ultrasonic frequency of 100kHz, after the ultrasonic dispersion is finished, adding organic resin emulsion with the solid content of 30 percent and the mass of graphene oxide of 10 percent, continuing to perform ultrasonic dispersion for 40 minutes at the ultrasonic frequency of 60kHz, performing suction filtration, collecting a filter cake, washing the filter cake for 3 times by using deionized water, transferring the washed filter cake into an oven, and drying to constant weight at the temperature of 100 ℃ to obtain a precursor; the organic resin emulsion is selected from styrene-acrylic emulsion;
transferring the precursor into a carbonization furnace, introducing nitrogen into the carbonization furnace at the speed of 10mL/min for protection, heating to 1300 ℃ at the speed of 5 ℃/min under the protection of nitrogen, carrying out heat preservation treatment for 2h, then continuously heating to 2200 ℃ at the speed of 10 ℃/min, carrying out heat preservation high-temperature graphitization treatment for 4h, then cooling to room temperature along with the furnace, and discharging to obtain graphene particles;
film forming by screen printing:
according to the weight parts, 30 parts of graphene particles, 150 parts of water-based acrylate emulsion with the solid content of 40%, 5 parts of absolute ethyl alcohol, 1 part of 1,3 butanediol and 10 parts of deionized water are sequentially taken, mixed, stirred and dispersed for 30min by a stirrer at the rotating speed of 1000r/min, and then carbon fibers are added, wherein the mass ratio of the carbon fibers to the graphene particles is 1:10, the length distribution range of the carbon fiber is 200-300 mu m; the aspect ratio of the carbon fiber is 20:1, after the carbon fibers are added, continuously stirring and dispersing for 10min at the rotating speed of 1000r/min by using a stirrer, and discharging to obtain basic slurry;
fixing a polyimide film serving as a base film, performing screen printing on the surface, controlling the using amount of basic slurry to 2900mL per square meter, after printing is finished, performing vacuum drying at 200 ℃ for 5min, cooling, discharging, and removing the film to obtain the product.
Example 2
Preparing graphene particles:
mixing graphene oxide with D50 of 400 mu m and deionized water according to a mass ratio of 1:7, performing ultrasonic dispersion for 3 hours at the temperature of 47 ℃ and the ultrasonic frequency of 110kHz, after the ultrasonic dispersion is finished, adding organic resin emulsion with the solid content of 40% and the mass of 15% of graphene oxide, continuing to perform ultrasonic dispersion for 60 minutes at the ultrasonic frequency of 70kHz, performing suction filtration, collecting a filter cake, washing the filter cake for 4 times by using deionized water, transferring the washed filter cake into a drying oven, and drying to constant weight at the temperature of 105 ℃ to obtain a precursor; the organic resin emulsion is selected from pure acrylic emulsion;
transferring the precursor into a carbonization furnace, introducing nitrogen into the carbonization furnace at a speed of 20mL/min for protection, heating to 1350 ℃ at a speed of 8 ℃/min under the protection of nitrogen, carrying out heat preservation treatment for 2h, then continuously heating to 2300 ℃ at a speed of 12 ℃/min, carrying out heat preservation high-temperature graphitization treatment for 5h, then cooling to room temperature along with the furnace, and discharging to obtain graphene particles;
film forming by screen printing:
according to the weight parts, 35 parts of graphene particles, 180 parts of water-based acrylate emulsion with the solid content of 42%, 8 parts of absolute ethyl alcohol, 2 parts of 1,3 butanediol and 15 parts of deionized water are sequentially taken, mixed, stirred and dispersed for 40min by a stirrer at the rotating speed of 1100r/min, and then carbon fibers are added, wherein the mass ratio of the carbon fibers to the graphene particles is 1:12, the length distribution range of the carbon fiber is 250-300 μm; the aspect ratio of the carbon fiber is 30:1, after the carbon fibers are added, continuously stirring and dispersing for 15min at the rotating speed of 1100r/min by using a stirrer, and discharging to obtain basic slurry;
fixing a polyimide film serving as a base film, performing screen printing on the surface, controlling the use amount of basic slurry to be 3200mL per square meter, after printing is finished, performing vacuum drying at 220 ℃ for 8min, cooling, discharging, and removing the film to obtain the product.
Example 3
Preparing graphene particles:
mixing graphene oxide with D50 of 600 mu m and deionized water according to a mass ratio of 1:8, performing ultrasonic dispersion for 4 hours at the temperature of 55 ℃ and the ultrasonic frequency of 120kHz, after the ultrasonic dispersion is finished, adding organic resin emulsion with the solid content of 50% and the mass of 20% of graphene oxide, continuing to perform ultrasonic dispersion for 80min at the ultrasonic frequency of 80kHz, performing suction filtration, collecting a filter cake, washing the filter cake for 5 times by using deionized water, transferring the washed filter cake into an oven, and drying to constant weight at the temperature of 110 ℃ to obtain a precursor; the organic resin emulsion is selected from silicone-acrylic emulsion;
transferring the precursor into a carbonization furnace, introducing nitrogen gas into the carbonization furnace at a speed of 30mL/min for protection, heating to 1400 ℃ at a speed of 10 ℃/min under the protection of nitrogen gas, carrying out heat preservation treatment for 3h, continuing heating to 2400 ℃ at a speed of 15 ℃/min, carrying out heat preservation high-temperature graphitization treatment for 6h, cooling to room temperature along with the furnace, and discharging to obtain graphene particles;
film forming by screen printing:
according to the weight parts, 40 parts of graphene particles, 200 parts of water-based acrylate emulsion with the solid content of 45%, 10 parts of absolute ethyl alcohol, 3 parts of 1,3 butanediol and 20 parts of deionized water are sequentially taken, mixed, stirred and dispersed for 50min by a stirrer at the rotating speed of 1200r/min, and then carbon fibers are added, wherein the mass ratio of the carbon fibers to the graphene particles is 1:15, the length distribution range of the carbon fiber is 200-280 μm; the aspect ratio of the carbon fiber is 40:1, after the carbon fibers are added, continuously stirring and dispersing for 30min at the rotating speed of 1200r/min by using a stirrer, and discharging to obtain basic slurry;
fixing a polyimide film serving as a base film, performing screen printing on the surface, controlling the use amount of basic slurry to be 4200 mL/square meter, after printing is finished, performing vacuum drying at 260 ℃ for 10min, cooling, discharging, and removing the film to obtain the product.
Example 4
This example differs from example 1 in that: the silicone-acrylic emulsion with equal mass is adopted to replace the styrene-acrylic emulsion, and the other conditions are kept unchanged.
Example 5
This example differs from example 1 in that: transferring the precursor into a carbonization furnace, introducing nitrogen into the carbonization furnace at a speed of 10mL/min for protection, directly heating to 2200 ℃ at a speed of 10 ℃/min under the protection of nitrogen, carrying out heat preservation and high-temperature graphitization treatment for 4 hours, cooling to room temperature along with the furnace, and discharging to obtain graphene particles; the remaining conditions remained unchanged.
Example 6
This example differs from example 1 in that: no carbon fiber was added and the remaining conditions were kept constant.
Comparative example 1
This comparative example is different from example 1 in that: adopting the substituted styrene-acrylic emulsion with the mass fraction of 5 percent of CMC dispersion liquid and the like, and keeping the rest conditions unchanged.
Blank example
This blank example differs from example 1 in that: the styrene-acrylic emulsion is not added, and the other conditions are kept unchanged.
The products obtained in examples 1-6, comparative example 1 and the blank example were subjected to performance tests, and the specific test methods and test results are as follows:
the thermal conductivity of the material was tested at room temperature (25 ℃) using a laser flash method. Firstly, respectively cutting the product into wafers with the diameter of 40mm, then placing the wafers into a mold of a thermal conductivity meter for testing, wherein the instrument used for testing is an LFA-467 thermal conductivity meter produced by Germany Chiari corporation, and the specific test results are shown in Table 1;
then, after the wafers obtained by cutting in different examples, comparative examples and blank examples are bent for 100 times at 90 degrees, the thermal conductivity of the wafers is tested again, and the specific test results are shown in table 1;
table 1: product performance test results
The test results in table 1 show that the product obtained by the invention has good heat-conducting property, and after being folded for many times, the product structure still keeps stable, the stability of the heat-conducting property of the product can be effectively kept, and the use scene of the product is effectively widened;
in addition, under the condition of room temperature, the product is cut into a rectangular membrane with the specification of 50 × 100cm, a thermocouple is adopted to heat the central point of the rectangular membrane, the temperature of the central point is controlled to be 80 ℃, and the temperature of the rectangular membrane after being heated for 60s is tested at four corners, wherein the specific test results are shown in table 2:
table 2: product performance test results
As can be seen from the test results in Table 2, the product obtained by the present invention has better uniformity in the heat transfer process.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A high performance graphene film comprising graphene particles; the graphene particles comprise layered graphene layers and spherical graphitized carbon microspheres embedded among the graphene layers;
moreover, the spherical graphitized carbon microspheres are hollow structures;
the preparation method of the graphene particles comprises the following steps:
dispersing graphene oxide in water, adding an organic resin emulsion with the solid content of 30-50%, performing ultrasonic dispersion uniformly, performing suction filtration, and drying to obtain a precursor;
carrying out high-temperature graphitization treatment on the precursor to obtain graphene particles;
the high-temperature graphitization treatment comprises the following steps: firstly, under the protection of inert gas, the precursor is subjected to heat preservation treatment for 2-3h at the temperature of 1000-1100 ℃, then the temperature is raised to 2200-2400 ℃, and high-temperature graphitization treatment is carried out for 4-6h;
the organic resin emulsion is selected from any one of styrene-acrylic emulsion, pure acrylic emulsion and silicone acrylic emulsion.
2. The high-performance graphene film according to claim 1, further comprising carbon fibers, wherein a mass ratio of the carbon fibers to the graphene particles is 1:10-1:15.
3. the high-performance graphene film according to claim 2, wherein the D50 of the graphene particles is 100-600 μ ι η; the length distribution range of the carbon fiber is 200-300 mu m; the aspect ratio of the carbon fiber is 20:1-40:1.
4. the graphene film according to claim 1, wherein the spherical graphitized carbon microspheres comprise silicon carbide.
5. The high-performance graphene film according to claim 1, further comprising a matrix resin, wherein the matrix resin is an aqueous acrylate.
6. The preparation method of the high-performance graphene film according to any one of claims 1 to 5, wherein the specific preparation steps comprise:
preparing graphene particles:
dispersing graphene oxide in water, adding an organic resin emulsion with the solid content of 30-50%, performing ultrasonic dispersion uniformly, performing suction filtration, and drying to obtain a precursor;
carrying out high-temperature graphitization treatment on the precursor to obtain graphene particles;
and (3) uniformly dispersing the graphene particles and the water-based acrylate emulsion, and then screen-printing to form a film, thus obtaining the product.
7. The method for preparing the high-performance graphene film according to claim 6, wherein the organic resin emulsion is selected from silicone acrylic emulsion.
8. The method of claim 6, wherein the screen printing to form the film comprises:
fixing polyimide film as base film, silk screen printing, vacuum drying at 200 deg.c for 5-10min, and discharging.
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| CN110642246A (en) * | 2018-06-26 | 2020-01-03 | 中国石油天然气股份有限公司 | Preparation method of graphene microspheres |
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| WO2018031064A1 (en) * | 2016-08-08 | 2018-02-15 | Nanotek Instruments, Inc. | Graphene oxide-bonded metal foil thin film current collector |
| CN106987188B (en) * | 2017-05-03 | 2020-02-28 | 杭州高烯科技有限公司 | Graphene-based water-based acrylic coating and preparation method thereof |
| CN108948886B (en) * | 2018-07-18 | 2020-10-30 | 杭州高烯科技有限公司 | Phase-change temperature-regulating coating and preparation method thereof |
| WO2020023578A1 (en) * | 2018-07-25 | 2020-01-30 | Global Graphene Group, Inc. | Chemical-free production of hollow graphene balls |
| CN111908452A (en) * | 2020-07-13 | 2020-11-10 | 深圳市展旺新材料科技有限公司 | Graphene carbon nanotube composite high-thermal-conductivity film and preparation method thereof |
| CN112898953B (en) * | 2021-01-14 | 2021-12-28 | 扬州晟至宝新材料科技有限公司 | Preparation method of graphene heat-conducting film |
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| CN108190866A (en) * | 2018-03-02 | 2018-06-22 | 山东大学 | A kind of method that water-in-oil emulsion method simply controls synthesis sea urchin shape graphene ball |
| CN110642246A (en) * | 2018-06-26 | 2020-01-03 | 中国石油天然气股份有限公司 | Preparation method of graphene microspheres |
| CN108928816A (en) * | 2018-07-23 | 2018-12-04 | 燕山大学 | A kind of N doping graphitized carbon microballoon and its preparation method and application with ultra-microporous |
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