CN115285978A - Preparation method of high-cohesion graphene heat-conducting film - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000005011 phenolic resin Substances 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 29
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005096 rolling process Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000005087 graphitization Methods 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 23
- 238000004321 preservation Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 10
- 230000017525 heat dissipation Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000007731 hot pressing Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 67
- 239000000463 material Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000009864 tensile test Methods 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 drying Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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Abstract
The invention relates to a preparation method of a high-cohesion graphene heat-conducting film, which comprises the steps of adding water-based phenolic resin powder into a water solution containing a surfactant to prepare a mixed system, and carrying out ultrasonic treatment to form a stable-dispersion emulsion; adding graphite oxide into deionized water for dispersion to prepare slurry, and dispersing to obtain graphene oxide slurry; mixing the emulsion and the graphene oxide slurry, and performing mixing treatment to obtain a graphene oxide/phenolic resin composite slurry; coating and drying the composite slurry to obtain a graphene oxide/phenolic resin composite film; carrying out hot pressing on the composite membrane to obtain a densified graphene oxide composite membrane, heating the composite membrane to 1200 ℃, preserving heat to finish carbonization, then heating the composite membrane to 3150 ℃, preserving heat to finish graphitization, and preparing to obtain the graphene oxide composite membrane with the density of 0.6-0.8g/cm 3 The graphene film of (1); further rolling and compacting until the density reaches 1.8-2.1g/cm 3 And obtaining the high-thermal-conductivity graphene heat dissipation film. The invention can effectively improve the internal molecular arrangement of grapheneAnd the cohesion and the heat conduction effect are improved.
Description
Technical Field
The invention relates to the field of graphene, in particular to a preparation method of a high-cohesion graphene heat-conducting film.
Background
With the rapid development of microelectronic integration technology, high power density electronic devices such as smart phones and tablet computers generate a large amount of heat, and the temperature of the working environment thereof is also increased rapidly, thereby affecting the working performance and the service life of the electronic devices. Particularly, with the coming of the 5G era, the operating power is 2-5 times that of 4G, the heat productivity is doubled, and higher requirements are put forward on heat dissipation materials.
The graphite heat dissipation film is a film-shaped material with ultra-high in-plane heat conductivity, and can quickly diffuse heat released by the chip in the plane to realize cooling. However, the current mature graphite heat dissipation film is prepared by carbonizing and graphitizing a PI film, the method has high requirements on raw materials, and only a thin PI film can obtain an artificial graphite film with high thermal conductivity, so that the product is generally below 25 micrometers, and a thicker graphite film is difficult to obtain. This results in graphite films with insufficient heat flux, difficulty in dissipating more heat, and further limited application, although the thermal conductivity can be as high as 1200W/(mK) or more.
The theoretical thermal conductivity coefficient of the single-layer graphene is about 5300W/(mK), which is higher than that of an artificial graphite film, and the single-layer graphene is an ideal thermal interface conducting material. In the prior art, a common idea is to prepare a high thermal conductivity graphene film by taking graphene oxide as a raw material and performing coating, drying, film forming, carbonization and graphitization processes. In patent CN 105860939A, a high thermal conductivity graphene film is prepared by coating graphene oxide, drying to form a film, soaking in a reducing agent for reduction, performing high-temperature heat treatment, rolling and compacting, and the like; in patent CN 106495133A, graphene oxide powder is mixed with a reducing agent to obtain graphene slurry, and the graphene slurry is coated, dried to form a film, and subjected to heat treatment to prepare a graphene film; in patent CN107555419A, graphene oxide is subjected to solution film forming, chemical reduction, low-temperature heat treatment, high-temperature hot pressing, and the like to obtain a graphene film with low wrinkle density. However, none of the above methods relate to a specific method for preparing a thicker graphene film. In patent CN103449423A, graphite oxide is ultrasonically dispersed in deionized water, and is coated to obtain a graphene oxide thin film, and the graphene oxide thin film is dried and reduced at high temperature to obtain a graphene heat conduction film, but in the method, reduction reaction is performed after coating of graphene oxide slurry, and the thickness of the finally obtained graphene film is limited and is less than 100 micrometers. Patent CN102573413A discloses a graphene heat dissipation film, which comprises a support layer, a graphene layer and an adhesive layer combined with each other, and can be used for manufacturing a multi-layer graphene heat dissipation film, but the process method is complex and has high cost.
Therefore, a method for preparing a multilayer graphene heat dissipation film with unlimited thickness at low cost and by a simpler process and a graphene heat conduction film prepared by the method are needed to be provided.
Disclosure of Invention
The invention aims to provide a preparation method of a high-cohesion graphene heat conduction film, which solves the problems of insufficient heat conduction coefficient and insufficient heat flux caused by weak cohesion of the existing graphite/graphene soaking film material, and further solves the problems of preparation of the high-cohesion graphite/graphene soaking film material by simplifying the existing complex process and reduction of cost.
The invention achieves the aim through the following technical scheme, and a first aspect provides a preparation method of a high-cohesion graphene heat-conducting film, which comprises the following steps: step S1, preparing phenolic resin emulsion; s2, adding a certain amount of graphite oxide into deionized water for dispersing to prepare slurry with the solid content of 2-6%, and performing ultrasonic treatment and stirring dispersion to obtain uniformly dispersed graphene oxide slurry; s3, fully mixing the emulsion obtained in the step S1 and the graphene oxide slurry obtained in the step S2, and treating the mixture by a homogenizer to obtain graphene oxide/phenolic resin composite slurry; step S4, coating the composite slurry obtained in the step S3 on a coating machine to form a film, and drying the film to obtain a graphene oxide/phenolic resin composite film; step S5, carbonizing and graphitizing the composite membrane obtained in the step S4 to obtain a graphene membrane; and S6, further rolling the graphene film obtained in the step S5 to obtain the high-cohesion graphene heat-conducting film.
According to an optional embodiment of the present invention, the configuration process of step S1 is: adding a predetermined amount of water-soluble phenolic resin into an aqueous solution containing a surfactant to prepare a mixed system with the mass percentage of the phenolic resin of 1-10%, and performing frosting treatment to form emulsion with stable dispersion.
According to an alternative embodiment of the present invention, the sanding treatment of step S1 is sanding the mixed system in a sand mill for 1-2 hours until the particle size reaches 100nm or less.
According to an alternative embodiment of the invention, the temperature of the mixed system during sanding in step S1 is kept below 22 ℃ or below 20 ℃.
According to an alternative embodiment of the invention, the mixing of step S3 is performed in a vacuum mixer for a mixing time of 1h.
According to an alternative embodiment of the invention, the homogenization conditions of step S3 are 2-3 passes at a pressure of 120 MPa.
According to an alternative embodiment of the invention, the coating thickness of step S4 is 2-10mm.
According to an alternative embodiment of the present invention, the carbonization treatment conditions of step S5 are such that carbonization is completed by raising the temperature at a rate of 5 ℃/min to a temperature in a first temperature range of 850 to 1200 ℃ and holding the temperature at the temperature in the first temperature range; then raising the temperature to a temperature within a second temperature range of 2800-3200 ℃ at a temperature of 20 ℃/min, preserving the heat at the temperature within the second temperature range to complete graphitization, and preparing the graphite with a density of 0.6-0.8g/cm 3 The graphene film of (1).
According to an alternative embodiment of the invention, it further comprises: heating to 1200 ℃ in a first temperature range; heating to 2850 ℃ or 3150 ℃ in a second temperature range; the heat preservation time of the heat preservation is 2 hours.
According to an optional embodiment of the present invention, in the step S6, the graphene film is compacted after being rolled until the density reaches 1.8 to 2.1g/cm 3 。
The invention achieves the above object by the following technical scheme, and the second aspect provides a high-cohesion graphene heat-conducting film obtained by the preparation method according to the first aspect.
Compared with the prior art, the preparation method of the high-cohesion graphene heat-conducting film and the prepared graphene heat-conducting film have the beneficial effects that: the graphene oxide and the aqueous phenolic resin powder are used for forming a film to form a more compact composite precursor, the aqueous phenolic resin powder has a good defect filling function, and the cohesion of the graphene can be effectively improved, so that the heat conduction path is improved, and the heat conduction effect is improved.
Particularly, the cohesion is strengthened, and the cohesion is obviously improved and the heat conductivity coefficient is improved by the deformation/peeling/tearing tensile test result tested by using a tensile testing machine, from about 1300 in the past to more than 1500 in the invention. In addition, wiping with a hand of graphene films or sheets of the prior art can result in sticking of the powder to the hand, which is not the case with the present invention.
Drawings
In order to make the technical problems solved, technical means adopted and technical effects achieved by the present invention clearer, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted, however, that the drawings described below are only illustrations of exemplary embodiments of the invention, from which other embodiments can be derived by those skilled in the art without inventive faculty.
Fig. 1 is a cohesion test of a graphene heat conduction film prepared without adding an aqueous phenolic resin powder.
Fig. 2 is a cohesion test condition of a graphene heat-conducting film prepared by adding aqueous phenolic resin powder in the preparation method of the high-cohesion graphene heat-conducting film according to the invention.
Detailed Description
Exemplary embodiments of the present invention will now be described more fully. The exemplary embodiments, however, may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these exemplary embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the invention to those skilled in the art.
The term "and/or" and/or "includes any and all combinations of one or more of the associated listed items.
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.
Example 1
A preparation method of a high-cohesion graphene heat-conducting film comprises the following steps:
step S1, adding a certain amount of water-based phenolic resin powder into a water solution containing a surfactant to prepare a mixed system with the mass percentage content of phenolic resin of 1-10%, sanding the mixed system in a sand mill for 2 hours until the granularity reaches below 100nm to form emulsion with stable dispersion, and keeping the temperature of the mixed system below 22 ℃ in the sanding process;
s2, adding a certain amount of graphite oxide into deionized water for dispersing to prepare slurry with the solid content of 2-6%, and dispersing by ultrasonic and stirring to obtain uniformly dispersed graphene oxide slurry;
step S3, fully mixing the emulsion obtained in the step S1 and the graphene oxide slurry obtained in the step S2 in a vacuum stirrer for 2 hours, preferably 1 hour, and treating for 2 times by a homogenizer under the pressure of 110-150 MPa, optionally 150MPa, so as to obtain the graphene oxide/phenolic resin composite slurry;
step S4, coating the composite slurry obtained in the step S3 on a coating machine to form a film, wherein the coating thickness is 2mm, and drying the film to form a film to obtain a graphene oxide/phenolic resin composite film, namely a graphene oxide and phenolic resin composite film;
s5, heating the composite membrane obtained in the step S4 to 850-1200 ℃, namely a first temperature range, preferably 1000 ℃, at a speed of 5 ℃/min, and preserving heat for 2 hours to finish carbonization; then heating to 2800-3200 deg.C (preferably 2850 deg.C) at 20 deg.C/min, and maintaining for 2 hr to complete graphitization to obtain graphite with density of 0.6-0.8g/cm 3 Preferably 0.6g/cm 3 ；
Step S6, further rolling the graphene film obtained in the step S5, and compacting until the density reaches 1.8-2.1g/cm 3 Preferably 1.8g/cm 3 And obtaining the high-cohesion graphene heat-conducting film.
Example 2
A preparation method of a high-cohesion graphene heat-conducting film comprises the following steps:
step S1, adding a certain amount of water-based phenolic resin powder into a water solution containing a surfactant to prepare a mixed system with the mass percentage content of the phenolic resin of 1-10%, preferably 10%, sanding the mixed system in a sand mill for 1-2h (h is a time unit hour), preferably 1.5 or 2h until the granularity reaches below 100nm, preferably 80nm, forming a stable dispersion emulsion, and keeping the temperature of the mixed system below 20 ℃ in the sanding process;
s2, adding a certain amount of graphite oxide into deionized water for dispersing to prepare slurry with the solid content of 2-6%, preferably 6%, and dispersing by ultrasonic and stirring to obtain uniformly dispersed graphene oxide slurry;
step S3, fully mixing the emulsion obtained in the step S1 and the graphene oxide slurry obtained in the step S2 in a vacuum stirrer for 1-2h, preferably for 2h, and treating the mixture for 2-3 times by a homogenizer under the pressure of 110-150 MPa, preferably for 3 times under the pressure of 120MPa to obtain graphene oxide/phenolic resin composite slurry;
step S4, coating the composite slurry obtained in the step S3 on a coating machine to form a film, wherein the coating thickness is 2-10mm, preferably 2mm, 4mm, 8mm and 10mm, and drying the film to form a film so as to obtain a graphene oxide/phenolic resin composite film;
s5, heating the composite membrane obtained in the step S4 to 850-1200 ℃, namely a first temperature range, preferably 1200 ℃, at a speed of 5 ℃/min, and preserving heat for 2h to finish carbonization; then heating to 2800-3500 deg.C (second temperature range) at 20 deg.C/min, preferably 3150 deg.C and 3200 deg.C, and maintaining for 2 hr to complete graphitization to obtain graphite with density of 0.6-0.8g/cm 3 Preferably 0.8g/cm 3 ；
Step S6, further rolling the graphene film obtained in the step S5, and compacting until the density reaches 1.8-2.1g/cm 3 Preferably 2.1g/cm 3 And obtaining the high-cohesion graphene heat-conducting film.
Comparative example 1
The phenol resin emulsion of step S1 was not added to the graphene oxide slurry, and the other steps were the same as in example 1. The prepared graphene heat-conducting film has poor cohesive force.
As can be seen from a comparison between fig. 1 and fig. 2, fig. 1 shows the cohesion test of the thermally conductive film obtained by the preparation method without adding the aqueous phenolic resin powder, and fig. 2 shows the high-cohesion thermally conductive film obtained by the method of the present invention, in which the cohesion is enhanced. In particular, the results of the deformation/peel/tear tensile test using a tensile tester show that the horizontal axis represents the deformation distance, i.e. the pulling to the corresponding deformation distance, and the vertical axis represents the required force, as can be seen in fig. 2 the force required for the material is significantly higher than in fig. 1, i.e. the cohesion is improved. Under the same test conditions, the average force in each interval of fig. 1, such as 21-24 gf, is significantly less than the average force in each interval of fig. 2, such as 31-34 gf, while the average force in the interval tested in the entirety of fig. 1, such as 22.831gf, is also less than the average force in the entirety of fig. 2, such as 33.855. Therefore, the preparation process disclosed by the invention is applied to the whole preparation flow by adding the water-based phenolic resin powder and matching with the emulsion generated by corresponding treatment, so that the prepared graphene heat-conducting film has high cohesive force, and the process is simple and easy to implement.
In addition, the graphene film or sheet of the prior art will stick to the hand when rubbed by hand, and the graphene film or sheet of the present invention will not stick to the hand when rubbed by hand.
Still further, based on the high flatness and weak interlayer of the graphene film, in combination with the large grain size of the graphene layer, the graphene film of the present invention obtains higher thermal conductivity and thermal conductivity, which is improved from about 1300 in the prior art to more than 1500 in the present invention.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (11)
1. A preparation method of a high-cohesion graphene heat-conducting film is characterized by comprising the following steps:
step S1, preparing phenolic resin emulsion;
s2, adding a certain amount of graphite oxide into deionized water for dispersing to prepare slurry with the solid content of 2-6%, and performing ultrasonic treatment and stirring dispersion to obtain uniformly dispersed graphene oxide slurry;
step S3, fully mixing the emulsion obtained in the step S1 and the graphene oxide slurry obtained in the step S2, and processing the mixture by a homogenizer to obtain graphene oxide/phenolic resin composite slurry;
step S4, coating the composite slurry obtained in the step S3 on a coating machine to form a film, and drying the film to obtain a graphene oxide/phenolic resin composite film;
step S5, carbonizing and graphitizing the composite membrane obtained in the step S4 to obtain a graphene membrane;
and S6, further rolling the graphene film obtained in the step S5 to obtain the high-cohesion graphene heat-conducting film.
2. The preparation method according to claim 1, wherein the configuration process of step S1 is:
adding a predetermined amount of water-soluble phenolic resin into an aqueous solution containing a surfactant to prepare a mixed system with the mass percentage of the phenolic resin of 1-10%, and performing sanding treatment to form emulsion with stable dispersion.
3. The method as claimed in claim 2, wherein the sanding treatment of step S1 is sanding the mixed system in a sand mill for 1-2 hours until the particle size reaches 100nm or less.
4. The method of claim 2, wherein the temperature of the mixed system is maintained below 22 ℃ or below 20 ℃ during the sanding of step S1.
5. The method of claim 1, wherein the mixing of step S3 is performed in a vacuum mixer for 1 hour.
6. The production method according to claim 1, wherein the homogenization treatment condition of the step S3 is treatment at a pressure of 120MPa for 2 to 3 times.
7. The method according to claim 1, wherein the coating thickness of step S4 is 2 to 10mm.
8. The method according to claim 1,
the carbonization treatment condition of the step S5 is that the temperature is raised to the temperature in a first temperature range of 850-1200 ℃ at the speed of 5 ℃/min, and the temperature is kept at the temperature in the first temperature range to finish carbonization;
then raising the temperature to the temperature in the second temperature range of 2800-3200 ℃ at the temperature of 20 ℃/min, preserving the heat at the temperature in the second temperature range, finishing graphitization, and preparing the graphite with the density of 0.6-0.8g/cm 3 The graphene film of (1).
9. The method of manufacturing according to claim 8, further comprising:
heating to 1200 ℃ in a first temperature range;
heating to 2850 ℃ or 3150 ℃ in a second temperature range;
the heat preservation time of the heat preservation is 2 hours.
10. The method according to claim 1, wherein in step S6, the graphene film is compacted to a density of 1.8 to 2.1g/cm after rolling 3 。
11. The high-cohesion graphene heat-conducting film obtained by the preparation method according to any one of claims 1 to 10.
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