CN115627073A - Wide artificial graphite high-conductivity film structure for communication base station - Google Patents

Wide artificial graphite high-conductivity film structure for communication base station Download PDF

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CN115627073A
CN115627073A CN202211344487.6A CN202211344487A CN115627073A CN 115627073 A CN115627073 A CN 115627073A CN 202211344487 A CN202211344487 A CN 202211344487A CN 115627073 A CN115627073 A CN 115627073A
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artificial graphite
base station
polyimide film
communication base
wide
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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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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
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    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/50Properties of the layers or laminate having particular mechanical properties
    • B32B2307/54Yield strength; Tensile strength
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    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract

The invention discloses a wide artificial graphite high-conductivity membrane structure for a communication base station, wherein a base material is a polyimide film, and the artificial graphite high-conductivity membrane structure is prepared by carbonizing and graphitizing the polyimide film, and is characterized in that the preparation of the polyimide film comprises the following steps: dissolving polyamic acid, wherein the mass percentage content of polyamic acid is 15-20%, adding carbon nano tubes, wherein the mass percentage of carbon nano tubes is 0.5-1.5%, performing ultrasonic dispersion after the addition is finished to prepare a precursor solution, and imidizing the prepared precursor solution and performing cold stretching treatment while imidizing. By adopting different addition agents and filler adding modes, the structure of the polyimide film is optimized, the graphene crystal can be better molded in the subsequent carbonization and graphitization processes, the sequencing directions of carbon atoms can be more ordered, and the ratio of the D peak intensity to the G peak intensity is far lower than that of the existing carbon film.

Description

Wide artificial graphite high-conductivity film structure for communication base station
Technical Field
The invention relates to a wide artificial graphite high-conductivity film structure for a communication base station.
Background
Unlike the general large base station, the small base station adopted by the new standard is often embedded in places such as office buildings, shopping malls, square flower beds and the like, and has the characteristics of miniaturization and heterogeneity. For example, common electronic devices have a temperature rise of 8-12 ℃, and a service life of the electronic devices is only about half of a normal operating temperature, so that a more efficient heat conduction structure is often required to ensure stable operation of a miniaturized base station.
In the inorganic non-metal heat conduction structure, the heat conduction capability of the graphite heat conduction film is most concerned, the main material of the existing artificial graphite high-conductivity film heat conduction structure is a polyimide film material, the polyimide film is widely applied to the fields of electronic and electrical, communication, military equipment manufacturing and the like and is also a 'gold film', the heat conduction requirement of the base station is gradually enhanced along with the continuous trial operation of new standards in the communication industry, and particularly when the base station runs at a high frequency or an ultra-high frequency, the base station needs a more excellent heat conduction system to maintain the stable running of the base station.
However, when the polyimide film is used for preparing high-performance products, the yield is low, the mechanical property fluctuation is large, the energy consumption is large, and the polyimide film still needs to be further optimized and improved in the preparation process of the high-performance products at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a wide artificial graphite high-conductivity film structure for a communication base station.
The utility model provides a high membrane structure that leads of wide range artificial graphite for communication base station, base material are the polyimide film, and the high membrane structure that leads of artificial graphite is prepared after carbonizing and graphitizing the polyimide film, the preparation of polyimide film includes following steps:
dissolving polyamic acid, wherein the mass percent of polyamic acid is 15-20%, adding carbon nano tubes, wherein the mass percent of carbon nano tubes is 0.5-1.5%, performing ultrasonic dispersion after the addition is finished to prepare a precursor solution, imidizing the prepared precursor solution, and performing cold stretching treatment while imidizing.
Furthermore, the diameter of the carbon nano tube is 10-25nm, and the length of the carbon nano tube is 5-15 μm.
In order to improve the growth efficiency of carbon crystals and the size of the crystals in the carbonization process and the graphitization process, a high-temperature resistant inorganic forming auxiliary agent is added in the imidization process, and the high-temperature resistant inorganic forming auxiliary agent is carbonate powder.
The specific adding mode of the inorganic forming auxiliary agent is that the viscosity of the precursor is adjusted during imidization, calcium carbonate powder is added when the viscosity is adjusted to 150 +/-10Pa.S by heating in water bath at 40-60 ℃, and ultrasonic oscillation is carried out to uniformly disperse the calcium carbonate powder in the slurry.
In order to further improve the performance of the polyimide film, inorganic filler can be supplemented before the polyimide film is formed so as to fill micropores and interlayer structures generated in the carbonization and graphitization processes of the polyimide film, and the interlayer spacing is improved so as to further improve the structural strength of the finished artificial graphite high-conductivity film, and the specific filler modification mode comprises the following steps: modifying the filler by adopting a silane coupling agent, adding the filler into the precursor solution in a protective atmosphere after modification, and fully stirring, wherein the using amount of the filler is not more than 1% of the mass of the precursor solution; the filler includes a ceramic-based filler and a metal-based filler.
Further, the ceramic filler is one of aluminum oxide, silicon dioxide, magnesium oxide or aluminum nitride.
Further, the metal filler is one or a mixture of several of gold powder, silver powder, aluminum powder and copper powder.
In order to protect the final artificial graphite high-conductivity membrane structure from being scratched by a sharp object, facilitate transportation and have better bending resistance in the use process, a layer of epoxy resin material is hot-pressed on the surface of the graphitized polyimide film, and the thickness of the epoxy resin material is 15% -18% of the total thickness of the artificial graphite high-conductivity membrane.
In the present invention, the specific way of dispersing the carbon nanotubes in the polyimide film is as follows:
1. at low temperature, diamine and dianhydride in the same molar amount are condensed in strong polar solvent to prepare polyamic acid, which is then added with carbon nanotube and imidized to obtain polyimide,
2. after the polyimide is obtained, the polyimide resin may be prepared into a powder, and the carbon nanotubes may be added to the polyimide resin and kneaded to obtain a polyimide film.
Both methods are used to disperse the carbon nanotubes in the polyimide film. The preparation process of the second mode is longer, but the improvement on the structural stability is better.
Has the advantages that:
this application carries out structural strength and performance optimization to the polyimide film through the form of homodisperse carbon nanotube in the polyimide film to make its graphite height that can prepare the width wideer lead membrane structure, so that use in the communication base station of equidimension not.
The polyimide film is structurally optimized by adopting different addition agents and filler adding modes, so that the graphene film can be better molded in the subsequent carbonization and graphitization processes, the ordering direction of carbon atoms can be more ordered, and the ratio of the D peak intensity to the G peak intensity is far lower than that of the existing carbon film.
Drawings
FIG. 1 is a graph showing the mass loss of polyimide films obtained by different processes in examples one to three;
FIG. 2 is a diagram of the maximum width range that can be made for different thicknesses while maintaining thermal conductivity above 1000.
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:
an artificial graphite high-conductivity structure, the substrate material of which is polyimide film, the preparation steps include the following steps:
dissolving polyamic acid, wherein the mass percent content of polyamic acid is 18%, adding carbon nano tubes, wherein the mass percent of the carbon nano tubes is 0.8%, adjusting the viscosity after the addition is finished, heating the mixture in water bath at 60 ℃, adding calcium carbonate powder when the viscosity is adjusted to 150 +/-10Pa.S, and performing ultrasonic oscillation to uniformly disperse the calcium carbonate powder in the slurry. The precursor solution was obtained, and cold stretching treatment was performed while imidizing and imidizing the prepared precursor solution.
Obtaining a polyimide film slice after cold stretching treatment and deflection, carbonizing and graphitizing the polyimide film, and thermally pressing a layer of epoxy resin material on the surface of the graphitized polyimide film, wherein the thickness of the epoxy resin material is 15% -18% of the total thickness of the artificial graphite high-conductivity film, and finally preparing the artificial graphite high-conductivity film structure.
Example two:
an artificial graphite high-conductivity structure, the substrate material of which is polyimide film, the preparation steps include the following steps:
dissolving polyamic acid, wherein the mass percent content of polyamic acid is 18%, adding carbon nano tubes, wherein the mass percent of the carbon nano tubes is 1%, adjusting the viscosity after the addition is finished, heating the mixture in water bath at 60 ℃, adding calcium carbonate powder when the viscosity is adjusted to 150 +/-10 Pa.S, and performing ultrasonic oscillation to uniformly disperse the calcium carbonate powder in the slurry. The precursor solution was obtained, and cold stretching treatment was performed while imidizing and imidizing the prepared precursor solution.
Obtaining a polyimide film slice after cold stretching treatment and deflection, carbonizing and graphitizing the polyimide film, and thermally pressing a layer of epoxy resin material on the surface of the graphitized polyimide film, wherein the thickness of the epoxy resin material is 15% -18% of the total thickness of the artificial graphite high-conductivity film, and finally preparing the artificial graphite high-conductivity film structure.
Example three:
an artificial graphite high-conductivity structure, the substrate material of which is polyimide film, the preparation steps include the following steps:
dissolving polyamic acid, wherein the mass percent content of polyamic acid is 18%, adding carbon nano tubes, wherein the mass percent of the carbon nano tubes is 1.2%, adjusting the viscosity after the addition is finished, heating the mixture in water bath at 60 ℃, adding calcium carbonate powder when the viscosity is adjusted to 150 +/-10Pa.S, and performing ultrasonic oscillation to uniformly disperse the calcium carbonate powder in the slurry. The precursor solution was obtained, and cold stretching treatment was performed while imidizing and imidizing the prepared precursor solution.
Obtaining a polyimide film slice after cold stretching treatment and deflection, carbonizing and graphitizing the polyimide film, and thermally pressing a layer of epoxy resin material on the surface of the graphitized polyimide film, wherein the thickness of the epoxy resin material is 15% -18% of the total thickness of the artificial graphite high-conductivity film, and finally preparing the artificial graphite high-conductivity film structure.
As can be seen from FIG. 2, by effectively pre-treating the polyimide film, the width range of the finished polyimide film after the carbon nanotubes are added can be effectively increased under the condition of different thickness dimensions on the premise of satisfying the kilowatt heat conductivity, so that the processing loss can be greatly reduced, and the processing efficiency can be improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.

Claims (8)

1. The utility model provides a membrane structure is led to wide width artificial graphite height for communication base station, the base material is the polyimide film, is carbonized and graphitizes the polyimide film after the preparation and obtains the membrane structure is led to artificial graphite height, its characterized in that, the preparation of polyimide film includes following step:
dissolving polyamic acid, wherein the mass percent of polyamic acid is 15-20%, adding carbon nano tubes, wherein the mass percent of carbon nano tubes is 0.5-1.5%, performing ultrasonic dispersion after the addition is finished to prepare a precursor solution, imidizing the prepared precursor solution, and performing cold stretching treatment while imidizing.
2. The wide-width artificial graphite high-conductivity film structure for the communication base station as claimed in claim 1, wherein the carbon nanotubes have a diameter of 10-25nm and a length of 5-15 μm.
3. The wide artificial graphite high-conductivity film structure for communication base station as claimed in claim 1, wherein a high temperature resistant inorganic forming aid is added during imidization, said high temperature resistant inorganic forming aid being carbonate powder.
4. The wide artificial graphite high-conductivity film structure for communication base station as claimed in claim 3, wherein the precursor is viscosity-adjusted during imidization, and calcium carbonate powder is added and subjected to ultrasonic vibration to uniformly disperse the calcium carbonate powder in the slurry when the viscosity is adjusted to 150 ± 10pa.s by heating in water bath at 40-60 ℃.
5. The wide-width artificial graphite high-conductivity film structure for the communication base station as claimed in claim 1, wherein silane coupling agent is used to modify the filler, and after modification, the filler is added into the precursor solution and fully stirred under the environment of protective atmosphere, wherein the usage amount of the filler is not more than 1% of the mass of the precursor solution; the filler includes a ceramic-based filler and a metal-based filler.
6. The wide-width artificial graphite high-conductivity film structure for communication base station as claimed in claim 5, wherein the ceramic filler is one of alumina, silica, magnesia or aluminum nitride.
7. The wide-width artificial graphite high-conductivity film structure for the communication base station as claimed in claim 5, wherein the metal filler is one or a mixture of gold powder, silver powder, aluminum powder and copper powder.
8. The wide artificial graphite high-conductivity film structure for the communication base station as claimed in claim 1, wherein a layer of epoxy resin material is hot-pressed on the surface of the graphitized polyimide film, and the thickness of the epoxy resin material is 15% -18% of the total thickness of the artificial graphite high-conductivity film.
CN202211344487.6A 2022-10-31 2022-10-31 Wide artificial graphite high-conductivity film structure for communication base station Pending CN115627073A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110423467A (en) * 2019-09-04 2019-11-08 株洲时代新材料科技股份有限公司 A kind of superthick polyimide film and preparation method thereof and graphite flake
CN110733153A (en) * 2019-09-17 2020-01-31 合肥领盛电子有限公司 method for manufacturing backboard of mobile phone
CN111470876A (en) * 2020-03-16 2020-07-31 中山大学 High-graphitization polyimide-based graphite thick film and preparation method thereof
CN112456484A (en) * 2019-12-27 2021-03-09 中天电子材料有限公司 Graphite heat-conducting film and preparation method thereof
WO2022086402A1 (en) * 2020-10-19 2022-04-28 Sht Smart High-Tech Ab Graphene film reinforced thermal conductive composite film and preparation method and use thereof
CN114523736A (en) * 2022-02-28 2022-05-24 安徽碳华新材料科技有限公司 High-performance artificial graphite high-conductivity film applied to heat dissipation structure

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110423467A (en) * 2019-09-04 2019-11-08 株洲时代新材料科技股份有限公司 A kind of superthick polyimide film and preparation method thereof and graphite flake
CN110733153A (en) * 2019-09-17 2020-01-31 合肥领盛电子有限公司 method for manufacturing backboard of mobile phone
CN112456484A (en) * 2019-12-27 2021-03-09 中天电子材料有限公司 Graphite heat-conducting film and preparation method thereof
CN111470876A (en) * 2020-03-16 2020-07-31 中山大学 High-graphitization polyimide-based graphite thick film and preparation method thereof
WO2022086402A1 (en) * 2020-10-19 2022-04-28 Sht Smart High-Tech Ab Graphene film reinforced thermal conductive composite film and preparation method and use thereof
CN114523736A (en) * 2022-02-28 2022-05-24 安徽碳华新材料科技有限公司 High-performance artificial graphite high-conductivity film applied to heat dissipation structure

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