CN112898953A - Preparation method of graphene heat-conducting film - Google Patents

Preparation method of graphene heat-conducting film Download PDF

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CN112898953A
CN112898953A CN202110046526.3A CN202110046526A CN112898953A CN 112898953 A CN112898953 A CN 112898953A CN 202110046526 A CN202110046526 A CN 202110046526A CN 112898953 A CN112898953 A CN 112898953A
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graphene
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CN112898953B (en
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蒋军良
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Yangzhou Shengzhi Baoxin Material Technology Co., Ltd
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Abstract

The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a graphene heat conduction film. The preparation method comprises the following steps: stirring and dissolving starch and water, then adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction, discharging, washing, and drying to obtain a starch-graphene hydrothermal carbon microsphere; stirring and dissolving glucose and water, then adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction, discharging, washing, and drying to obtain glucose-graphene hydrothermal carbon microspheres; mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres, taking a glycerol and ethylene glycol mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, adding 1 part of the glycerol and ethylene glycol mixture, stirring at a high viscosity, adding 3 parts of the glycerol and ethylene glycol mixture, stirring continuously, adding the rest 6 parts of the glycerol and ethylene glycol mixture, stirring and mixing uniformly, casting to form a film, drying, and uncovering the film to obtain the graphene heat-conducting film.

Description

Preparation method of graphene heat-conducting film
Technical Field
The invention belongs to the technical field of heat conduction materials. More particularly, the invention relates to a preparation method of a graphene heat conduction film.
Background
Heat conduction and heat dissipation have important application requirements in many fields such as electronics, communication, illumination, aviation, national defense and military industry and the like. The mainstream heat conducting materials in the market are still mainly aluminum and copper metal or alloy, and in recent ten years, graphite heat conducting films are widely applied and rapidly occupy the market share of the traditional materials. The graphite heat-conducting film has the following advantages: the heat conductivity coefficient is higher than 300-1500W/m.K and higher than that of various alloys and simple substance copper materials of aluminum; meanwhile, the weight of the alloy is 25 percent lighter than that of aluminum and 75 percent lighter than that of copper; and is convenient for cutting and cutting, and is convenient for use.
The thermally conductive graphite film is also known as a thermally conductive graphite sheet, a heat dissipating graphite film, a graphite heat dissipating film, or the like. The heat-conducting graphite film is a novel heat-conducting and heat-dissipating material, and the heat-conducting and heat-dissipating effect is very obvious. Low-dimensional carbon nanomaterials, such as graphene and carbon nanotubes, have thermal conductivities as high as 3000-6000W/m.K due to their extremely high elastic constants and mean free paths. The Graphene (Graphene) has the thickness of only 0.335nm, and has an ultra-large specific surface area, excellent electric and thermal conductivity and good chemical stability. These good properties make graphene-based materials an ideal thermal conducting material.
Balandin et al have measured thermal conductivity of single-layer graphene as high as 5300W/m.K, higher than 3000-3500W/m.K thermal conductivity of carbon nanotubes, by non-contact optical methods. Defects in graphene, edge disorder, etc. all reduce the thermal conductivity in graphene, and Ghosh et al measure the thermal conductivity of 1-10 layers of graphene, and find that the thermal conductivity decreases from 2800W/m · K to 1300W/m · K as the number of model layers increases from 2 to 4. The graphene heat-conducting film has high heat conduction coefficient and good stability at high temperature, and can be used as an efficient heat-radiating material. Most of the existing heat-conducting films are graphite and polyimide or graphene-graphite composite heat-radiating films, and compared with pure graphene heat-conducting films, the heat-conducting films are complex in preparation process, low in heat conductivity and high in cost. The conventional heat-conducting film still has the problem that the heat-conducting property cannot be further improved, so that research on the conventional heat-conducting film is needed.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings that the heat conducting performance of the existing graphene heat conducting film is rapidly reduced easily due to the increase of the number of graphene layers when heat is transferred in graphene due to gaps among the graphene layers, and provides a preparation method of the graphene heat conducting film.
The invention aims to provide a preparation method of a graphene heat-conducting film.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene heat conduction film comprises the following specific preparation steps:
(1) stirring and dissolving starch and water, adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction at the temperature of 180-200 ℃, discharging, washing, and drying to obtain starch-graphene hydrothermal carbon microspheres;
(2) stirring and dissolving glucose and water, then adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction at the temperature of 180 ℃ and 200 ℃, discharging, washing, and drying to obtain glucose-graphene hydrothermal carbon microspheres;
(3) according to the mass ratio of 3: 1-10: 1, mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres to obtain a mixture, taking a glycerol and ethylene glycol mixture with the mass of 0.3-0.5 times of that of the mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, adding 1 part of the glycerol and ethylene glycol mixture into the mixture, stirring at a high viscosity, adding 3 parts of the glycerol and ethylene glycol mixture, continuing stirring, adding the rest 6 parts of the glycerol and ethylene glycol mixture, and uniformly stirring and mixing to obtain a film forming solution;
(4) and (3) casting the film forming solution into a film, drying, and uncovering the film to obtain the graphene heat conducting film.
According to the technical scheme, the starch and glucose hydrothermal carbon microspheres are used for coating the graphene oxide, in the coating process, the layered structure of the graphene oxide is dispersed and then coated by the hydrothermal carbon microspheres, the edges of the layered structure are in contact with the wall surfaces of the hydrothermal carbon microspheres, in the heat conduction process, heat is conducted to the edges of the layered structure of the graphene oxide through the wall surfaces of the hydrothermal carbon microspheres, the layered structure quickly transfers the heat in the hydrothermal carbon microspheres, and at the moment, the heat can be directly transferred to the opposite surface of the wall surfaces of the hydrothermal carbon microspheres from the surface of a single sheet layer without passing through the space between the graphene layer and the graphene layer, so that the heat can be quickly transferred in the heat conduction membrane, and the heat conduction efficiency is effectively improved;
in addition, according to the technical scheme, the high-molecular polysaccharide (starch) and the monosaccharide (glucose) are respectively used as carbon sources, and can form hydrothermal carbon microspheres with different sizes in a hydrothermal process, and constraint forces with different sizes can be generated on an internally-coated graphene lamellar structure in a product preparation process, so that the graphene lamellar structure generates orientation structures in different directions inside, on one hand, the two hydrothermal carbon microspheres with different sizes are mixed, a particle grading effect can be generated, the density of a heat conduction network for forming a film is effectively improved, and heat transfer is accelerated; on the other hand, due to different orientations of graphene lamellar structures in the hydrothermal carbon microspheres, high heat transfer effects can be achieved in heat transfer in different directions.
Further, in the specific preparation steps of the graphene thermal conductive film, the step (4) further includes:
and (3) casting the film forming solution into a film, spraying a mixture of fatty acid and silicate ester, hot-pressing, drying, and uncovering the film to obtain the graphene heat conducting film.
Above-mentioned technical scheme further sprays fatty acid and silicate ester mixture to the product after the casting film-forming, and utilize the heat of hot pressing, make fatty acid and ethylene glycol take place dehydration condensation, and use silicate ester as water absorption catalyst, after silicate ester absorbed moisture, can hydrolyze and produce silicon dioxide, in case there is the silicon dioxide crystal nucleus to produce, can adsorb fixedly by hydrothermal carbon microsphere, thereby realize the packing to carbon microsphere pore structure, the inside density of further having improved the product, the porosity has been reduced, thereby the heat transfer effect has been promoted.
Further, the glycerol and diethanol mixture is prepared by mixing glycerol and ethylene glycol according to a mass ratio of 1: 1-1: 5 are compounded.
Further, the fatty acid and silicate ester mixture is prepared by mixing fatty acid and silicate ester according to a mass ratio of 1: 1-1: 3 is prepared by compounding.
Further, the fatty acid is any one selected from stearic acid, arachidonic acid, ricinoleic acid, linoleic acid and linolenic acid.
Further, the silicate is selected from any one of methyl orthosilicate, ethyl orthosilicate and isopropyl orthosilicate.
Further, the hot pressing is as follows: continuously hot pressing at 85-95 deg.C and 0.3-0.5MPa for 10-30 min.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Taking 10 parts of starch, 100 parts of water and 4 parts of graphene oxide in sequence according to parts by weight, mixing the starch and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by a stirrer at a rotating speed of 300r/min, then adding the graphene oxide, carrying out ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 60kHz, carrying out hydrothermal reaction for 18h under the conditions that the temperature is 180 ℃ and the stirring rotating speed is 400r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 3 times by deionized water, then transferring the washed filter cake into an oven, and drying the filter cake to constant weight under the condition that the temperature is 100 ℃ to obtain the starch-graphene hydrothermal carbon microspheres;
taking 10 parts of glucose, 100 parts of water and 4 parts of graphene oxide in sequence according to parts by weight, mixing the glucose and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by using a stirrer at a rotating speed of 300r/min, then adding the graphene oxide, carrying out ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 60kHz, carrying out hydrothermal reaction for 18h under the conditions that the temperature is 180 ℃ and the stirring rotating speed is 400r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 3 times by using deionized water, then transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 100 ℃ to obtain the glucose-graphene hydrothermal carbon microsphere;
according to the mass ratio of 3: 1, mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres, pouring the mixture into a mixer, stirring and mixing the mixture for 30min by using a stirrer under the condition of 200r/min to obtain a mixture, taking a glycerol and ethylene glycol mixture with the mass being 0.3 times of that of the mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, firstly adding 1 part of the glycerol and ethylene glycol mixture into the mixture, stirring the mixture at a high viscosity for 1h under the condition that the stirring speed is 300r/min, then adding 3 parts of the glycerol and ethylene glycol mixture, continuously stirring the mixture at a speed of 800r/min for 1h, then adding the remaining 6 parts of the glycerol and ethylene glycol mixture, and stirring and mixing the mixture for 1h under the condition that the rotating speed is 2000r/min to obtain a membrane forming solution;
after the film-forming liquid is casted into a film, spraying a mixture of fatty acid and silicate ester on the surface of the casted film-forming liquid, continuously hot-pressing for 10min at the temperature of 85 ℃ and the pressure of 0.3MPa, drying to constant weight at the temperature of 100 ℃, and uncovering the film to obtain the graphene heat-conducting film; the glycerol and diethanol mixture is prepared from glycerol and ethylene glycol according to a mass ratio of 1: 1 is compounded; the fatty acid and silicate ester mixture is prepared by mixing fatty acid and silicate ester according to the mass ratio of 1: 1 is compounded; the fatty acid is selected from stearic acid; the silicate is selected from methyl orthosilicate.
Example 2
Taking 20 parts of starch, 120 parts of water and 5 parts of graphene oxide in sequence according to parts by weight, mixing the starch and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by a stirrer at a rotating speed of 400r/min, adding the graphene oxide, performing ultrasonic dispersion for 20min under the condition that the ultrasonic frequency is 70kHz, performing hydrothermal reaction for 20h under the conditions that the temperature is 190 ℃ and the stirring rotating speed is 500r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 4 times by deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 105 ℃ to obtain the starch-graphene hydrothermal carbon microspheres;
taking 20 parts of glucose, 120 parts of water and 5 parts of graphene oxide in sequence according to parts by weight, mixing the glucose and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by using a stirrer at a rotating speed of 400r/min, then adding the graphene oxide, performing ultrasonic dispersion for 20min under the condition that the ultrasonic frequency is 70kHz, performing hydrothermal reaction for 20h under the conditions that the temperature is 190 ℃ and the stirring rotating speed is 500r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 4 times by using deionized water, then transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 105 ℃ to obtain the glucose-graphene hydrothermal carbon microspheres;
according to the mass ratio of 8: 1, mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres, pouring the mixture into a mixer, stirring and mixing for 50min by using a stirrer at 300r/min to obtain a mixture, taking a glycerol and ethylene glycol mixture with the mass being 0.4 times of that of the mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, firstly adding 1 part of the glycerol and ethylene glycol mixture into the mixture, stirring for 2h at a high viscosity under the condition that the stirring speed is 400r/min, then adding 3 parts of the glycerol and ethylene glycol mixture, continuing stirring for 2h at a speed of 1000r/min, then adding the remaining 6 parts of the glycerol and ethylene glycol mixture, and stirring and mixing for 2h at a speed of 2500r/min to obtain a membrane forming solution;
after the film-forming solution is casted into a film, spraying a mixture of fatty acid and silicate ester on the surface of the casted film-forming solution, continuously hot-pressing for 20min at the temperature of 90 ℃ and the pressure of 0.4MPa, drying to constant weight at the temperature of 102 ℃, and uncovering the film to obtain the graphene heat-conducting film; the glycerol and diethanol mixture is prepared from glycerol and ethylene glycol according to a mass ratio of 1: 3, compounding; the fatty acid and silicate ester mixture is prepared by mixing fatty acid and silicate ester according to the mass ratio of 1: 2, compounding; the fatty acid is selected from arachidonic acid; the silicate is selected from ethyl orthosilicate.
Example 3
Taking 30 parts of starch, 150 parts of water and 10 parts of graphene oxide in sequence according to parts by weight, mixing the starch and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by using a stirrer at the rotating speed of 500r/min, then adding the graphene oxide, carrying out ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 80kHz, carrying out hydrothermal reaction for 24h under the conditions that the temperature is 200 ℃ and the stirring rotating speed is 600r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 5 times by using deionized water, then transferring the washed filter cake into an oven, and drying the filter cake to constant weight under the condition that the temperature is 110 ℃ to obtain the starch-graphene hydrothermal carbon microspheres;
taking 30 parts of glucose, 150 parts of water and 10 parts of graphene oxide in sequence according to parts by weight, mixing the glucose and the water, pouring the mixture into a hydrothermal reaction kettle, stirring and dissolving the mixture by using a stirrer at the rotating speed of 500r/min, then adding the graphene oxide, carrying out ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 80kHz, carrying out hydrothermal reaction for 24h under the conditions that the temperature is 200 ℃ and the stirring rotating speed is 600r/min, discharging, filtering, collecting a filter cake, washing the filter cake for 5 times by using deionized water, then transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 110 ℃ to obtain the glucose-graphene hydrothermal carbon microsphere;
according to the mass ratio of 10: 1, mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres, pouring the mixture into a mixer, stirring and mixing for 60min by a stirrer under the condition of 400r/min to obtain a mixture, taking a glycerol and ethylene glycol mixture with the mass being 0.5 times of that of the mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, firstly adding 1 part of the glycerol and ethylene glycol mixture into the mixture, stirring for 3h at a high viscosity under the condition that the stirring speed is 500r/min, then adding 3 parts of the glycerol and ethylene glycol mixture, continuing stirring for 3h at the rotation speed of 1200r/min, then adding the rest 6 parts of the glycerol and ethylene glycol mixture, and stirring and mixing for 3h under the condition that the rotation speed is 3000r/min to obtain a membrane forming solution;
after the film-forming solution is casted into a film, spraying a mixture of fatty acid and silicate ester on the surface of the casted film-forming solution, continuously hot-pressing for 30min at the temperature of 95 ℃ and the pressure of 0.5MPa, drying to constant weight at the temperature of 105 ℃, and uncovering the film to obtain the graphene heat-conducting film; the glycerol and diethanol mixture is prepared from glycerol and ethylene glycol according to a mass ratio of 1: 5, compounding; the fatty acid and silicate ester mixture is prepared by mixing fatty acid and silicate ester according to the mass ratio of 1: 3, compounding; the fatty acid is selected from ricinoleic acid; the silicate is selected from isopropyl n-silicate.
Example 4
This example differs from example 1 in that: the surface of the cast film-forming solution was not sprayed with fatty acid and silicate, and the rest conditions were kept unchanged.
Comparative example 1
Compared with example 1, the glucose-graphene hydrothermal carbon microspheres are not added in the comparative example, and the rest conditions are kept unchanged.
Comparative example 2
Compared with example 1, the starch-graphene hydrothermal carbon microspheres are not added in the comparative example, and the rest conditions are kept unchanged.
Comparative example 3
Pouring graphene oxide into a mixer, taking a mixture of glycerol and glycol with the mass 0.3 time that of the graphene oxide, equally dividing the mixture of glycerol and glycol into 10 parts, firstly adding 1 part of the mixture of glycerol and glycol into the mixer, stirring for 1 hour at a stirring speed of 300r/min under high viscosity, then adding 3 parts of the mixture of glycerol and glycol, continuing stirring for 1 hour at a rotating speed of 800r/min, adding the rest 6 parts of the mixture of glycerol and glycol, and stirring and mixing for 1 hour at a rotating speed of 2000r/min to obtain a film-forming solution;
after the film-forming liquid is casted into a film, spraying a mixture of fatty acid and silicate ester on the surface of the casted film-forming liquid, continuously hot-pressing for 10min at the temperature of 85 ℃ and the pressure of 0.3MPa, drying to constant weight at the temperature of 100 ℃, and uncovering the film to obtain the graphene heat-conducting film; the glycerol and diethanol mixture is prepared from glycerol and ethylene glycol according to a mass ratio of 1: 1 is compounded; the fatty acid and silicate ester mixture is prepared by mixing fatty acid and silicate ester according to the mass ratio of 1: 1 is compounded; the fatty acid is selected from stearic acid; the silicate is selected from methyl orthosilicate.
The products obtained in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests, and the specific test methods and test results were as follows:
the above-mentioned examples and comparative examples were prepared into circular test specimens having a diameter of 10cm, and the in-plane thermal conductivity 1 of the test specimens and the Z-direction thermal conductivity 2 of the test specimens were respectively measured by a laser pulse method, and the specific test results are shown in table 1:
table 1: test result of heat conductivity of product
Thermal conductivity 1/W/(m.K) Thermal conductivity 2/W/(m.K)
Example 1 2450 1890
Example 2 2460 1920
Example 3 2455 1910
Example 4 2300 1850
Comparative example 1 1560 860
Comparative example 2 1550 850
Comparative example 3 1820 680
From the test results in table 1, it can be seen that the in-plane thermal conductivity and the Z-direction thermal conductivity of the product obtained by the present invention are excellent.
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 (7)

1. A preparation method of a graphene heat-conducting film is characterized by comprising the following specific preparation steps:
(1) stirring and dissolving starch and water, adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction at the temperature of 180-200 ℃, discharging, washing, and drying to obtain starch-graphene hydrothermal carbon microspheres;
(2) stirring and dissolving glucose and water, then adding graphene oxide, performing ultrasonic dispersion uniformly, performing hydrothermal reaction at the temperature of 180 ℃ and 200 ℃, discharging, washing, and drying to obtain glucose-graphene hydrothermal carbon microspheres;
(3) according to the mass ratio of 3: 1-10: 1, mixing starch-graphene hydrothermal carbon microspheres and glucose-graphene hydrothermal carbon microspheres to obtain a mixture, taking a glycerol and ethylene glycol mixture with the mass of 0.3-0.5 times of that of the mixture, equally dividing the glycerol and ethylene glycol mixture into 10 parts, adding 1 part of the glycerol and ethylene glycol mixture into the mixture, stirring at a high viscosity, adding 3 parts of the glycerol and ethylene glycol mixture, continuing stirring, adding the rest 6 parts of the glycerol and ethylene glycol mixture, and uniformly stirring and mixing to obtain a film forming solution;
(4) and (3) casting the film forming solution into a film, drying, and uncovering the film to obtain the graphene heat conducting film.
2. The method according to claim 1, wherein in the specific step of preparing the graphene thermal conductive film, the step (4) further comprises:
and (3) casting the film forming solution into a film, spraying a mixture of fatty acid and silicate ester, hot-pressing, drying, and uncovering the film to obtain the graphene heat conducting film.
3. The method for preparing the graphene thermal conductive film according to claim 1, wherein the mixture of glycerol and diethanol is prepared from glycerol and ethylene glycol in a mass ratio of 1: 1-1: 5 are compounded.
4. The method for preparing the graphene thermal conductive film according to claim 2, wherein the mixture of the fatty acid and the silicate is prepared by mixing the fatty acid and the silicate in a mass ratio of 1: 1-1: 3 is prepared by compounding.
5. The method according to claim 4, wherein the fatty acid is any one selected from stearic acid, arachidonic acid, ricinoleic acid, linoleic acid, and linolenic acid.
6. The method according to claim 4, wherein the silicate is selected from any one of methyl orthosilicate, ethyl orthosilicate, and isopropyl orthosilicate.
7. The method for preparing the graphene thermal conductive film according to claim 4, wherein the hot pressing is: continuously hot pressing at 85-95 deg.C and 0.3-0.5MPa for 10-30 min.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114957897A (en) * 2022-06-27 2022-08-30 苏福(深圳)科技有限公司 High-performance graphene film and preparation method thereof

Citations (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120097923A1 (en) * 2010-09-17 2012-04-26 Institute of Microelectronics, Chinese Academy of Sciences Graphene device and method for manufacturing the same
CN102544459A (en) * 2012-01-09 2012-07-04 上海交通大学 Method for preparing graphene-coated carbon microsphere material by coating graphene oxide on carbon microsphere
CN102881898A (en) * 2012-09-17 2013-01-16 上海交通大学 Preparation method and application of carbon-coated grapheme-based metal oxide composite
CN103804942A (en) * 2014-02-12 2014-05-21 厦门凯纳石墨烯技术有限公司 Graphene-containing insulated radiating composition and preparation and application thereof
CN103805144A (en) * 2014-03-04 2014-05-21 中国科学院宁波材料技术与工程研究所 Graphene heat conducting film and preparation method thereof
CN105036124A (en) * 2015-08-22 2015-11-11 苏州正业昌智能科技有限公司 Method for preparing graphene from polysaccharide
CN106513694A (en) * 2016-12-14 2017-03-22 中国航空工业集团公司北京航空材料研究院 Preparation method of graphene/ metal composite powder
CN107140631A (en) * 2017-06-09 2017-09-08 哈尔滨工业大学 A kind of preparation method of the super-hydrophobic graphene film of bionic intelligence
CN107161980A (en) * 2017-05-24 2017-09-15 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 A kind of preparation method of the carbon nanosheet with graphene oxide fold pattern
CN107381549A (en) * 2017-07-31 2017-11-24 常州市天宁区鑫发织造有限公司 A kind of preparation method of graphene heat conducting film
CN107674228A (en) * 2017-09-30 2018-02-09 湖南国盛石墨科技有限公司 The preparation method of graphene heat conducting film
CN108622885A (en) * 2018-07-06 2018-10-09 青岛大学 A kind of preparation method of graphene film
CN108658615A (en) * 2018-06-14 2018-10-16 华南理工大学 A kind of graphene-based laminated film of high heat conduction and preparation method thereof
CN108823601A (en) * 2018-07-06 2018-11-16 青岛大学 A kind of preparation method of metal oxide/graphene composite film
CN109824033A (en) * 2019-03-06 2019-05-31 华南理工大学 A kind of method of low cost preparation high thermal conductivity graphene film
CN109913289A (en) * 2019-03-25 2019-06-21 陕西科技大学 A kind of preparation method of graphene oxide cladding carbosphere composite material

Patent Citations (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120097923A1 (en) * 2010-09-17 2012-04-26 Institute of Microelectronics, Chinese Academy of Sciences Graphene device and method for manufacturing the same
CN102544459A (en) * 2012-01-09 2012-07-04 上海交通大学 Method for preparing graphene-coated carbon microsphere material by coating graphene oxide on carbon microsphere
CN102881898A (en) * 2012-09-17 2013-01-16 上海交通大学 Preparation method and application of carbon-coated grapheme-based metal oxide composite
CN103804942A (en) * 2014-02-12 2014-05-21 厦门凯纳石墨烯技术有限公司 Graphene-containing insulated radiating composition and preparation and application thereof
CN103805144A (en) * 2014-03-04 2014-05-21 中国科学院宁波材料技术与工程研究所 Graphene heat conducting film and preparation method thereof
CN105036124A (en) * 2015-08-22 2015-11-11 苏州正业昌智能科技有限公司 Method for preparing graphene from polysaccharide
CN106513694A (en) * 2016-12-14 2017-03-22 中国航空工业集团公司北京航空材料研究院 Preparation method of graphene/ metal composite powder
CN107161980A (en) * 2017-05-24 2017-09-15 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 A kind of preparation method of the carbon nanosheet with graphene oxide fold pattern
CN107140631A (en) * 2017-06-09 2017-09-08 哈尔滨工业大学 A kind of preparation method of the super-hydrophobic graphene film of bionic intelligence
CN107381549A (en) * 2017-07-31 2017-11-24 常州市天宁区鑫发织造有限公司 A kind of preparation method of graphene heat conducting film
CN107674228A (en) * 2017-09-30 2018-02-09 湖南国盛石墨科技有限公司 The preparation method of graphene heat conducting film
CN108658615A (en) * 2018-06-14 2018-10-16 华南理工大学 A kind of graphene-based laminated film of high heat conduction and preparation method thereof
CN108622885A (en) * 2018-07-06 2018-10-09 青岛大学 A kind of preparation method of graphene film
CN108823601A (en) * 2018-07-06 2018-11-16 青岛大学 A kind of preparation method of metal oxide/graphene composite film
CN109824033A (en) * 2019-03-06 2019-05-31 华南理工大学 A kind of method of low cost preparation high thermal conductivity graphene film
CN109913289A (en) * 2019-03-25 2019-06-21 陕西科技大学 A kind of preparation method of graphene oxide cladding carbosphere composite material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114957897A (en) * 2022-06-27 2022-08-30 苏福(深圳)科技有限公司 High-performance graphene film and preparation method thereof

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