CN114574167A - Preparation method of low-leakage high-heat-conduction graphene heat dissipation film - Google Patents

Preparation method of low-leakage high-heat-conduction graphene heat dissipation film Download PDF

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CN114574167A
CN114574167A CN202210329243.4A CN202210329243A CN114574167A CN 114574167 A CN114574167 A CN 114574167A CN 202210329243 A CN202210329243 A CN 202210329243A CN 114574167 A CN114574167 A CN 114574167A
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graphene
heat dissipation
dissipation film
heat
change material
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杨云胜
郭颢
束国法
蒋伟良
陈玲
陶勇
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Anhui Carbon China New Material Technology Co ltd
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Anhui Carbon China New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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  • Ceramic Engineering (AREA)
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Abstract

The invention discloses a preparation method of a low-leakage high-heat-conduction graphene heat dissipation film, which comprises the following steps: modifying graphene by adopting a Hummers method, and preparing a powdery graphene material; carrying out high-temperature melting treatment on the phase-change material, and adding the powdery graphene after melting; after adding the powdery graphene, performing first ultrasonic stirring, coating the powdery graphene on the upper surface of the glass, and allowing the lower surface of the glass to pass through normal-temperature cooling water; repeating the step of S5 for multiple times until a plurality of flaky semi-finished materials are prepared; spin-coating silicone oil on the surface of the semi-finished product material, and laminating, wherein the specific total thickness of the lamination is determined by the use requirement; the phase-changeable graphene heat dissipation film is prepared through a hot-press molding process. This product adds graphite alkene material in traditional phase change material to through the mode of layering coating, carry out the layering with graphite alkene material, graphite alkene material is with the quick leading-in phase change material's of heat inside, thereby lets the quick heat absorption of phase change material.

Description

Preparation method of low-leakage high-heat-conduction graphene heat dissipation film
Technical Field
The invention relates to a preparation method of a low-leakage high-heat-conduction graphene heat dissipation film.
Background
The phase-change material can absorb or release heat from an external environment by utilizing a self-reversible phase-change process, so that the storage or release of the heat is realized, and the phase-change material has the advantages of high energy storage density, stable temperature and the like.
In some special scenes, such as a chip heat dissipation scene using short time and high power, the internal space is small, so that heat cannot be conducted out in an effective heat dissipation mode, especially in scenes with high safety requirements, such as the weapon control field, the requirement of the chip heat dissipation scene is that heat cannot be dissipated outwards in a centralized manner, otherwise the chip heat dissipation scene can be monitored by infrared detection.
In such a field where a large amount of heat is instantaneously generated and heat cannot be instantaneously transferred, but instantaneous heat needs to be collected and slowly discharged, the phase change material has good adaptability.
The graphene material has excellent heat conduction performance, and if the graphene material is applied to a phase-change heat-absorbing material, the heat absorption and heat conduction capability of the phase-change heat-absorbing material can be improved, so that the phase-change heat-absorbing material has the capability of instantly absorbing a large amount of heat.
Disclosure of Invention
In order to overcome the defects of the prior art, a preparation method of a low-leakage high-heat-conduction graphene heat dissipation film is provided.
A preparation method of a low-leakage high-heat-conduction graphene heat dissipation film comprises the following steps:
s1, modifying the graphene by a Hummers method, and after modification is completed, performing modification according to the following steps of 1: 5-1: 6 mixing the graphene powderAnd KMnO4Mixing, and fully mixing in a sulfuric acid/phosphoric acid mixed solution in an ice bath environment;
s2, mixing, stirring for 12 hours at 50 ℃, filtering the mixed solution by a screen, cleaning and centrifuging for multiple times;
s3, performing condensation and suction filtration by using ether, performing quaternization treatment on the product in a nitrogen environment, and performing ultrasonic dispersion, washing, filtering, vacuum drying and grinding to obtain powdery graphene;
s4, carrying out high-temperature melting treatment on the phase change material, and adding the powdery graphene after melting;
s5, adding the powdered graphene, performing first ultrasonic stirring, coating the mixture on the upper surface of the glass, and cooling the lower surface of the glass with normal-temperature cooling water;
s6, repeating the steps S5 for multiple times until a plurality of flaky semi-finished materials are prepared;
s7, spin-coating silicone oil on the surface of the semi-finished product material, and laminating, wherein the specific total thickness of the laminated layer is determined by the use requirement;
s8, preparing the phase-changeable graphene heat dissipation film through a hot-press molding process.
Further, the thickness of the semi-finished product material is less than 0.15 mm.
Further, the phase change material is a nylon 6 phase change material prepared by coaxial electrostatic spinning, and the melting point is 32.2 ℃.
Furthermore, polytetrafluoroethylene protective layers are coated on the upper surface and the lower surface of the graphene heat dissipation film, and polytetrafluoroethylene wires interwoven in a warp-weft mode are arranged on the surfaces of the graphene heat dissipation film.
In order to prevent the materials from overflowing in a molten state, the polytetrafluoroethylene wire is woven in a warp-weft interweaving mode, after weaving is completed, the distance between every two adjacent warps is 0.01-0.15mm, the distance between every two adjacent wefts is 0.5-1.2 times of the distance between every two adjacent warps, after winding is completed, the warps and the wefts on the side faces are embedded between the graphene heat dissipation films in a hot-pressing mode, and the warps and the wefts on the front face and the back face are embedded in the polytetrafluoroethylene protective layers.
Has the advantages that:
phase change materials are often used for energy storage, but the characteristics that the phase change materials can absorb a large amount of heat and slowly release the heat can be utilized, so that the application of local heat dissipation of components and parts by utilizing the phase change principle is prepared.
This product adds graphite alkene material in traditional phase change material to through the mode of layering coating, carry out the layering setting with graphite alkene material, thereby great promotion whole phase change material's heat absorption efficiency, when contacting with the heat source, graphite alkene material is with the quick leading-in of heat in phase change material's inside, thereby let the quick heat absorption of phase change material, improved the slow disadvantage of traditional phase change material heat absorption, thereby can be arranged in the quick heat conduction of components and parts with phase change material.
Drawings
Fig. 1 is a modified preparation method of graphene powder.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
The first embodiment is as follows:
a preparation method of a low-leakage high-heat-conduction graphene heat dissipation film;
the method comprises the following steps:
s1, modifying the graphene by a Hummers method, and after modification is completed, performing modification according to the following steps of 1: 5-1: 6, mixing the graphene powder and the KMnO4Mixing, and fully mixing in a sulfuric acid/phosphoric acid mixed solution in an ice bath environment, wherein the specific reaction process is shown in figure 1;
s2, mixing, stirring for 12 hours at the temperature of 50 ℃, filtering the mixed solution by a screen, cleaning and centrifuging twice;
s3, performing condensation and suction filtration by using ether, performing quaternization treatment on the product in a nitrogen environment, and performing ultrasonic dispersion, washing, filtering, vacuum drying and grinding to obtain powdery graphene;
s4, performing high-temperature melting treatment on the phase change material, and adding the powdery graphene after melting;
s5, adding the powdery graphene, performing first ultrasonic stirring, coating the mixture on the upper surface of the glass, and allowing the lower surface of the glass to pass through normal-temperature cooling water;
s6, repeating the steps in the S5 for multiple times until 15 flaky semi-finished materials are prepared, wherein the thickness of the semi-finished materials is 0.1 mm;
s7, spin-coating silicone oil on the surface of the semi-finished product material, and laminating, wherein the specific total thickness of the laminated layer is determined by the use requirement;
s8, preparing the phase-changeable graphene heat dissipation film through a hot-press molding process.
S9, coating polytetrafluoroethylene protective layers on the upper surface and the lower surface of the graphene heat dissipation film, and arranging polytetrafluoroethylene wires interwoven in a warp-weft mode on the surfaces of the graphene heat dissipation film;
s10, weaving the polytetrafluoroethylene wire in a warp-weft interweaving mode, enabling the distance between every two adjacent warps to be 0.15mm after weaving, enabling the distance between every two adjacent wefts to be 0.1 times of the distance between every two adjacent warps, embedding the warps and the wefts on the side surfaces between the graphene heat dissipation films in a hot pressing mode after winding, and embedding the warps and the wefts on the front surface and the back surface in the polytetrafluoroethylene protective layers.
Example two:
a preparation method of a low-leakage high-heat-conduction graphene heat dissipation film;
the method comprises the following steps:
s1, modifying the graphene by a Hummers method, and after modification is completed, performing modification according to the following steps of 1: 5-1: 6, mixing the graphene powder and the KMnO4Mixing, and fully mixing in a sulfuric acid/phosphoric acid mixed solution in an ice bath environment, wherein the specific reaction process is shown in figure 1;
s2, mixing, stirring for 12 hours at the temperature of 50 ℃, filtering the mixed solution by a screen, cleaning and centrifuging twice;
s3, performing condensation and suction filtration by using ether, performing quaternization treatment on the product in a nitrogen environment, and performing ultrasonic dispersion, washing, filtering, vacuum drying and grinding to obtain powdery graphene;
s4, performing high-temperature melting treatment on the phase change material, and adding the powdery graphene after melting;
s5, adding the powdery graphene, performing first ultrasonic stirring, coating the mixture on the upper surface of the glass, and allowing the lower surface of the glass to pass through normal-temperature cooling water;
s6, repeating the steps in the S5 for multiple times until 20 flaky semi-finished materials are prepared, wherein the thickness of the semi-finished materials is 0.08 mm;
s7, spin-coating silicone oil on the surface of the semi-finished product material, and laminating, wherein the specific total thickness of the laminated layer is determined by the use requirement;
s8, preparing the phase-changeable graphene heat dissipation film through a hot-press molding process.
S9, coating polytetrafluoroethylene protective layers on the upper surface and the lower surface of the graphene heat dissipation film, and arranging polytetrafluoroethylene wires interwoven in a warp-weft mode on the surfaces of the graphene heat dissipation film;
s10, weaving the polytetrafluoroethylene wires in a warp-weft interweaving mode, enabling the distance between every two adjacent warps to be 0.15mm and the distance between every two adjacent wefts to be 0.15mm after weaving, embedding the warps and the wefts on the side surfaces between the graphene heat dissipation films in a hot pressing mode after winding, and embedding the warps and the wefts on the front surface and the back surface in the polytetrafluoroethylene protective layers.
As a further improvement, the above-mentioned is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A preparation method of a low-leakage high-heat-conduction graphene heat dissipation film is characterized by comprising the following steps:
s1, modifying the graphene by a Hummers method, and after modification is completed, performing modification according to the following steps of 1: 5-1: 6, mixing the graphene powder and the KMnO4Mixing, and fully mixing in a sulfuric acid/phosphoric acid mixed solution in an ice bath environment;
s2, mixing, stirring for 12 hours at 50 ℃, filtering the mixed solution by a screen, cleaning and centrifuging for multiple times;
s3, performing condensation and suction filtration by using ether, performing quaternization treatment on the product in a nitrogen environment, and performing ultrasonic dispersion, washing, filtering, vacuum drying and grinding to obtain powdery graphene;
s4, performing high-temperature melting treatment on the phase change material, and adding the powdery graphene after melting;
s5, adding the powdery graphene, performing first ultrasonic stirring, coating the mixture on the upper surface of the glass, and allowing the lower surface of the glass to pass through normal-temperature cooling water;
s6, repeating the step S5 for multiple times until a plurality of flaky semi-finished materials are prepared;
s7, spin-coating silicone oil on the surface of the semi-finished product material, and laminating, wherein the specific total thickness of the laminated layer is determined by the use requirement;
s8, preparing the phase-changeable graphene heat dissipation film through a hot-press molding process.
2. The method as claimed in claim 1, wherein the thickness of the semi-finished material is less than 0.15 mm.
3. The method for preparing a low-leakage high-thermal-conductivity graphene heat dissipation film according to claim 1, wherein the phase change material is a nylon 6 phase change material prepared by coaxial electrospinning, and has a melting point of 32.2 ℃.
4. The method for preparing a low-leakage high-thermal-conductivity graphene heat dissipation film according to claim 1, wherein polytetrafluoroethylene protection layers are coated on the upper surface and the lower surface of the graphene heat dissipation film, and polytetrafluoroethylene wires interwoven with warps and wefts are arranged on the surfaces of the graphene heat dissipation film.
5. The method for preparing a low-leakage high-thermal-conductivity graphene heat dissipation film according to claim 4, wherein polytetrafluoroethylene wires are woven in a warp-weft interweaving manner, after weaving is completed, the distance between adjacent warps is 0.01-0.15mm, the distance between adjacent wefts is 0.5-1.2 times the distance between adjacent warps, after winding is completed, the warps and wefts on the side surfaces are embedded between the graphene heat dissipation films in a hot-pressing manner through hot pressing, and the warps and wefts on the front and back surfaces are embedded in the polytetrafluoroethylene protection layer.
CN202210329243.4A 2022-03-31 2022-03-31 Preparation method of low-leakage high-heat-conduction graphene heat dissipation film Pending CN114574167A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150026670A (en) * 2013-08-30 2015-03-11 주식회사 서환이지 Heat dissipation sheet using graphite for electronic device
CN106861449A (en) * 2017-03-08 2017-06-20 中国海洋大学 A kind of quaternary ammoniated graphene oxide composite nano filter membrane and preparation method thereof
CN107564874A (en) * 2017-08-21 2018-01-09 硕阳科技股份公司 A kind of flexible heat sink film and preparation method thereof and composite and flexible radiating film
CN110753480A (en) * 2019-10-29 2020-02-04 Oppo广东移动通信有限公司 Heat radiating fin, preparation method thereof and electronic equipment

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150026670A (en) * 2013-08-30 2015-03-11 주식회사 서환이지 Heat dissipation sheet using graphite for electronic device
CN106861449A (en) * 2017-03-08 2017-06-20 中国海洋大学 A kind of quaternary ammoniated graphene oxide composite nano filter membrane and preparation method thereof
CN107564874A (en) * 2017-08-21 2018-01-09 硕阳科技股份公司 A kind of flexible heat sink film and preparation method thereof and composite and flexible radiating film
CN110753480A (en) * 2019-10-29 2020-02-04 Oppo广东移动通信有限公司 Heat radiating fin, preparation method thereof and electronic equipment

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