CN104023505A - Method for preparing high thermal conductivity graphite film - Google Patents
Method for preparing high thermal conductivity graphite film Download PDFInfo
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- CN104023505A CN104023505A CN201410260879.3A CN201410260879A CN104023505A CN 104023505 A CN104023505 A CN 104023505A CN 201410260879 A CN201410260879 A CN 201410260879A CN 104023505 A CN104023505 A CN 104023505A
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Abstract
The invention relates to heat dissipation film materials applied to electron components, in particular to a method for preparing a high thermal conductivity graphite film. Graphene powder and silicon carbide nano particles are used as raw materials, a polyimide film is obtained by adding molecular modifiers, and then the graphite film is obtained through carbonization, graphitization and rolling. Generation of defects in the carbonation process is reduced due to the laminated structure of graphene, the graphitization degree is improved due to the existence of the silicon carbide nano particles, and the quality of graphite film materials is further improved.
Description
Technical field
The present invention relates to a kind of the heat dissipation film material that is applied to electronic devices and components, particularly a kind of preparation method of high conductive graphite film.
Background technology
Along with developing rapidly of microelectronics integrated technology and high density PCB packaging technology, packaging density improves rapidly, and electronic component, thousands of times of ground of logical circuit volume dwindle, and electronic instrument and equipment are day by day towards light, thin, short, little future development.Under high-frequency work frequency, semiconductor working heat environment moves rapidly to high temperature direction, now, heat run-up, increase that electronic devices and components produce, at environment for use temperature, electronic devices and components still can normally be worked on high reliability ground, and heat-sinking capability becomes the critical limitation in its useful life factor that affects in time.For ensureing components and parts operational reliability, need to use the material of the excellent combination properties such as high reliability, high thermal conductivity, rapidly, the heat that in time heater element gathered passes to heat dissipation equipment, ensures that electronic equipment normally moves.Dissimilar heat sink material can have different performances, such as the heat conductivility of metal is good, a part of metal material wherein particularly, as copper, aluminium, silver etc., utilize these metal radiators as copper radiator, the radiator of aluminum, obtain general application.Due to scientific and technological development, above-mentioned metal material is processed and cannot have been met the highly integrated requirement of electron trade as heat carrier, thereby there is the Delanium membrane material of high heat dispersion, its thermal conductivity is very high, there is good flexibility, thereby be expected to be applied in heat transfer device material and radiator material that narrow place maybe needs the place that processes through gap always.But present high conductive graphite film also has weak point, although high heat conducting film has certain folding resistance, the weak strength between material, can be torn easily, or because of the displacement at the position that adheres to, disrepair phenomenon occurs.How effectively to increase the thermal diffusivity of heat conducting film, increasing its resistance to bend(ing) energy simultaneously and reducing process energy consumption is current urgent problem.
Summary of the invention
Technical barrier to be solved by this invention is, overcomes the deficiencies in the prior art, and a kind of preparation method of high conductive graphite film is provided, and prepared graphite film has efficient heat conductivility and excellent bending resistance.
Technical solution of the present invention is, take graphene powder and nanometer silicon carbide particle is raw material, adds molecular modification agent and obtains polyimide film; Then through carbonization, graphitization, calendering makes graphite film.
Concrete technology step is as follows:
(1) graphene powder and nanometer silicon carbide particle are dissolved in absolute ethyl alcohol, through ultrasonic agitation, 30～60min obtains mixed solution.
(2), under the condition of 50～70 ℃ of water-baths, in above-mentioned mixed solution, add molecular modification agent, return stirring 4～6h, under the centrifugation rate of 5000～9000rpm/min, carry out centrifugal, with ethanol washing, at 50～80 ℃, be dried, obtain the nano-grain of modification.
(3) 25～60g, 4,4 ＇-diaminodiphenyl ether is dissolved in organic polar solvent, passes into inert gas, stir 2～5h, then add 30～80g 3,3,4,4-tetracarboxylic benzophenone acid anhydride, continues to stir 3～5h, obtains PAA solution.
(4) then in PAA solution, add the nano-grain of modification described in step (2), the mixing speed stirring 5～20min with 5000～8000rpm/min in the inert atmosphere of 0～10 ℃ carries out home position polymerization reaction.
(5) solution after polymerization reaction is laid on substrate, uses after electron beam heating 1～3h, obtain polyimide composite film.
(6) select polyimide composite film as raw material, intersect stackingly, be positioned in carbide furnace and carry out carbonization, then the complete material of carbonization is moved in graphitizing furnace and carry out again graphitization, take out calendering.
Molecular modification agent described in step (2) is one or more mixtures in KH550, KH570 or amino silicane coupling agent.
Organic polar solvent described in step (3) is one or more mixtures in DMF, DMA and METHYLPYRROLIDONE.
Inert gas described in step (3) is a kind of in argon gas or helium.
Substrate described in step (5) is glass plate.
Compared with prior art, the advantage possessing is in the present invention:
1. because Graphene is two-dimentional lamellar structure as thin as a wafer, as reinforcing material, be distributed in material system, can be effectively and matrix have an effect, form plane and netted interconnected enhancing system, stop the defect forming due to chemical constitution change in carbonisation, improved the quality of heat conduction carbon film.
2. in the process of high temperature graphitization, catalyzed graphitization effect has been played in adding of nanometer silicon carbide particle, has improved degree of graphitization and has increased the toughness of heat conducting film.
Embodiment
Below the preferred embodiments of the present invention are described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention are made to more explicit defining.
Embodiment 1
The nano material first Graphene and silicon-carbide particle being mixed is dissolved in absolute ethyl alcohol, and ultrasonic agitation 30min obtains mixed solution.Under the condition of 50 ℃ of water-baths, in mixed solution (1), add molecular modification agent, return stirring 4, under the centrifugation rate of 5000rpm/min, carry out centrifugal, with ethanol washing, 50 ℃ dry, obtain the nano-grain of modifier modification.25g 4,4 ＇-diaminodiphenyl ether is dissolved in organic polar solvent again, passes into inert gas, stir 2h, then add 30g 3,3,4,4-tetracarboxylic benzophenone acid anhydride, continues to stir 3h, obtains PAA solution.In solution (3), add nano-grain, the mixing speed stirring 5min with 5000rpm/min in the inert atmosphere of 2 ℃ carries out in-situ polymerization, and reaction 3h, obtains solution X.Solution X is laid on clean substrate, uses electron beam heating, power 0.7KW, radiation dose rate 50Gy/s, obtain polyimide composite film after time 1h.Finally select polyimide film as raw material, intersect stackingly, be positioned in carbide furnace and within the regular hour, be warming up to carburizing temperature, carry out carbonization, then the complete material of carbonization is moved in graphitizing furnace and carry out graphitization, take out calendering.Make artificial conductive graphite film, conductive coefficient is 1800 W/mk.
Embodiment 2
The nano material first Graphene and silicon-carbide particle being mixed is dissolved in absolute ethyl alcohol, and ultrasonic agitation 50min obtains mixed solution.Under the condition of 60 ℃ of water-baths, in mixed solution (1), add molecular modification agent, return stirring 5h, under the centrifugation rate of 7000rpm/min, carry out centrifugal, with ethanol washing, 70 ℃ dry, obtain the nano-grain of modifier modification.50g 4,4 ＇-diaminodiphenyl ether is dissolved in organic polar solvent again, passes into inert gas, stir 4h, then add 60g 3,3,4,4-tetracarboxylic benzophenone acid anhydride, continues to stir 4h, obtains PAA solution.Then in solution (3), add nano-grain, the mixing speed stirring 15min with 7000rpm/min in the inert atmosphere of 5 ℃ carries out in-situ polymerization, and reaction 7h, obtains solution X.Solution X is laid on clean substrate, solution X is laid on clean substrate, use electron beam heating, power 0.7KW, radiation dose rate 50Gy/s, obtain polyimide composite film after time 2h.Finally select polyimide film as raw material, intersect stackingly, be positioned in carbide furnace and within the regular hour, be warming up to carburizing temperature, carry out carbonization, then the complete material of carbonization is moved in graphitizing furnace and carry out graphitization, take out calendering.Make artificial conductive graphite film, conductive coefficient is 1857 W/mk.
Embodiment 3
The nano material first Graphene and silicon-carbide particle being mixed is dissolved in absolute ethyl alcohol, and ultrasonic agitation 60min obtains mixed solution.Under the condition of 70 ℃ of water-baths, in mixed solution (1), add molecular modification agent, return stirring 6h, under the centrifugation rate of 7000rpm/min, carry out centrifugal, with ethanol washing, 70 ℃ dry, obtain the nano-grain of modifier modification.60g 4,4 ＇-diaminodiphenyl ether is dissolved in organic polar solvent again, passes into inert gas, stir 5h, then add 80g 3,3,4,4-tetracarboxylic benzophenone acid anhydride, continues to stir 5h, obtains PAA solution.Then in solution (3), add nano-grain, the mixing speed stirring 20min with 8000rpm/min in the inert atmosphere of 10 ℃ carries out in-situ polymerization, and reaction 8h, obtains solution X.Solution X is laid on clean substrate, solution X is laid on clean substrate, use electron beam heating, power 0.7KW, radiation dose rate 50Gy/s, obtain polyimide composite film after time 3h.Finally select polyimide film as raw material, intersect stackingly, be positioned in carbide furnace and within the regular hour, be warming up to carburizing temperature, carry out carbonization, then the complete material of carbonization is moved in graphitizing furnace and carry out graphitization, take out calendering.Make artificial conductive graphite film, conductive coefficient is 1920 W/mk.
Claims (6)
1. a preparation method for high conductive graphite film, is characterized in that: take graphene powder and nanometer silicon carbide particle is raw material, adds molecular modification agent and obtains polyimide film; Then through carbonization, graphitization, calendering makes graphite film.
2. the preparation method of a kind of high conductive graphite film as claimed in claim 1, is characterized in that: concrete technology step is as follows:
(1) graphene powder and nanometer silicon carbide particle are dissolved in absolute ethyl alcohol, through ultrasonic agitation, 30～60min obtains mixed solution;
(2), under the condition of 50～70 ℃ of water-baths, in above-mentioned mixed solution, add molecular modification agent, return stirring 4～6h, under the centrifugation rate of 5000～9000rpm/min, carry out centrifugal, with ethanol washing, at 50～80 ℃, be dried, obtain the nano-grain of modification;
(3) 25～60g, 4,4 ＇-diaminodiphenyl ether is dissolved in organic polar solvent, passes into inert gas, stir 2～5h, then add 30～80g 3,3,4,4-tetracarboxylic benzophenone acid anhydride, continues to stir 3～5h, obtains PAA solution;
(4) then in PAA solution, add the nano-grain of modification described in step (2), the mixing speed stirring 5～20min with 5000～8000rpm/min in the inert atmosphere of 0～10 ℃ carries out home position polymerization reaction;
(5) solution after polymerization reaction is laid on substrate, uses after electron beam heating 1～3h, obtain polyimide composite film;
(6) select polyimide composite film as raw material, intersect stackingly, be positioned in carbide furnace and carry out carbonization, then the complete material of carbonization is moved in graphitizing furnace and carry out again graphitization, take out calendering.
3. the preparation method of a kind of high conductive graphite film as claimed in claim 2, is characterized in that: the molecular modification agent described in step (2) is one or more mixtures in KH550, KH570 or amino silicane coupling agent.
4. the preparation method of a kind of high conductive graphite film as claimed in claim 2, it is characterized in that: the organic polar solvent described in step (3) is N, one or more mixtures in dinethylformamide, DMA and METHYLPYRROLIDONE.
5. the preparation method of a kind of high conductive graphite film as claimed in claim 2, is characterized in that: the inert gas described in step (3) is a kind of in argon gas or helium.
6. the preparation method of a kind of high conductive graphite film as claimed in claim 2, is characterized in that: the substrate described in step (5) is glass plate.
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| CN201410260879.3A CN104023505A (en) | 2014-06-13 | 2014-06-13 | Method for preparing high thermal conductivity graphite film |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592950A (en) * | 2014-12-26 | 2015-05-06 | 苏州格瑞丰纳米科技有限公司 | High-thermal conductivity graphite alkenyl polymer heat conducting film and preparation method thereof |
| CN106744792A (en) * | 2016-12-01 | 2017-05-31 | 达迈科技股份有限公司 | For rolling up the graphited polyimide film of burning formula and graphite film manufacturing method |
| CN107265451A (en) * | 2017-07-17 | 2017-10-20 | 安徽国风塑业股份有限公司 | A kind of preparation method of the polyimides graphite film of high conductive high strength |
| CN107383873A (en) * | 2017-08-03 | 2017-11-24 | 上海理工大学 | A kind of graphene/polyimide composite film and preparation method thereof |
| CN107804843A (en) * | 2017-11-20 | 2018-03-16 | 苏州世华新材料科技有限公司 | A kind of preparation technology of uniformly high heat conduction graphite film coiled material |
| CN110304625A (en) * | 2019-06-25 | 2019-10-08 | 浙江福斯特新材料研究院有限公司 | Graphene induces the preparation method of the high thermal conductivity graphite film of orientation of polyimide crystallization |
| CN110606950A (en) * | 2019-09-26 | 2019-12-24 | 宁波墨西科技有限公司 | Preparation method of PEI (polyetherimide) composite material |
| CN112322834A (en) * | 2020-09-29 | 2021-02-05 | 南京钢铁股份有限公司 | Bismuth-manganese-iron alloy core-spun yarn |
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| US20070232734A1 (en) * | 2006-03-31 | 2007-10-04 | Karthikeyan Kanakarajan | Polyimide based compositions useful in high frequency circuitry applications and methods relating thereto |
| CN102838106A (en) * | 2012-09-26 | 2012-12-26 | 哈尔滨工业大学 | Method for preparing carbon film by using silicon carbide-enhanced polyimide composite film |
| CN103011141A (en) * | 2012-12-20 | 2013-04-03 | 宁波今山新材料有限公司 | Method for manufacturing high thermal conductivity graphite film |
| CN103194058A (en) * | 2013-04-08 | 2013-07-10 | 桂林电子科技大学 | High-thermal-conductive moisture permeable film and preparation method thereof |
| CN103374224A (en) * | 2012-04-13 | 2013-10-30 | 达胜科技股份有限公司 | Polyimide film, method for producing same, and polyimide film laminate comprising same |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20070232734A1 (en) * | 2006-03-31 | 2007-10-04 | Karthikeyan Kanakarajan | Polyimide based compositions useful in high frequency circuitry applications and methods relating thereto |
| CN103374224A (en) * | 2012-04-13 | 2013-10-30 | 达胜科技股份有限公司 | Polyimide film, method for producing same, and polyimide film laminate comprising same |
| CN102838106A (en) * | 2012-09-26 | 2012-12-26 | 哈尔滨工业大学 | Method for preparing carbon film by using silicon carbide-enhanced polyimide composite film |
| CN103011141A (en) * | 2012-12-20 | 2013-04-03 | 宁波今山新材料有限公司 | Method for manufacturing high thermal conductivity graphite film |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592950A (en) * | 2014-12-26 | 2015-05-06 | 苏州格瑞丰纳米科技有限公司 | High-thermal conductivity graphite alkenyl polymer heat conducting film and preparation method thereof |
| CN106744792A (en) * | 2016-12-01 | 2017-05-31 | 达迈科技股份有限公司 | For rolling up the graphited polyimide film of burning formula and graphite film manufacturing method |
| CN107265451A (en) * | 2017-07-17 | 2017-10-20 | 安徽国风塑业股份有限公司 | A kind of preparation method of the polyimides graphite film of high conductive high strength |
| CN107383873A (en) * | 2017-08-03 | 2017-11-24 | 上海理工大学 | A kind of graphene/polyimide composite film and preparation method thereof |
| CN107804843A (en) * | 2017-11-20 | 2018-03-16 | 苏州世华新材料科技有限公司 | A kind of preparation technology of uniformly high heat conduction graphite film coiled material |
| CN107804843B (en) * | 2017-11-20 | 2018-07-10 | 苏州世华新材料科技有限公司 | A kind of preparation process of uniform high heat conduction graphite film coiled material |
| CN110304625A (en) * | 2019-06-25 | 2019-10-08 | 浙江福斯特新材料研究院有限公司 | Graphene induces the preparation method of the high thermal conductivity graphite film of orientation of polyimide crystallization |
| CN110606950A (en) * | 2019-09-26 | 2019-12-24 | 宁波墨西科技有限公司 | Preparation method of PEI (polyetherimide) composite material |
| CN110606950B (en) * | 2019-09-26 | 2021-11-02 | 宁波墨西科技有限公司 | Preparation method of PEI (polyetherimide) composite material |
| CN112322834A (en) * | 2020-09-29 | 2021-02-05 | 南京钢铁股份有限公司 | Bismuth-manganese-iron alloy core-spun yarn |
| CN112322834B (en) * | 2020-09-29 | 2022-06-17 | 南京钢铁股份有限公司 | Bismuth-manganese-iron alloy core-spun yarn |
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Application publication date: 20140903 |