CN104495798A - Manufacturing method of graphite heat-conduction membrane - Google Patents
Manufacturing method of graphite heat-conduction membrane Download PDFInfo
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- CN104495798A CN104495798A CN201410700634.8A CN201410700634A CN104495798A CN 104495798 A CN104495798 A CN 104495798A CN 201410700634 A CN201410700634 A CN 201410700634A CN 104495798 A CN104495798 A CN 104495798A
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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
- C01B32/20—Graphite
- C01B32/205—Preparation
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- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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Abstract
The invention relates to a manufacturing method of a graphite heat-conduction membrane. The manufacturing method comprises the following steps of 1, carrying out plasma treatment on a polyimide film, 2, arranging the 3-50 polyimide films treated by the step 1 between two graphite papers, and carrying out heating treatment to obtain a crystalline carbon foam film and 3, carrying out rolling or lamination so that the crystalline carbon foam film is processed to form the graphite heat-conduction membrane with the smooth surface. Compared with the existing manufacturing method, the manufacturing method improves production power by 1-5 times and has a stable yield rate. The graphite heat-conduction membrane has the soft and smooth surface and has no adverse surface and a heat conduction coefficient more than 1800w/(m.k). The heat conduction coefficient of the graphite heat-conduction membrane is higher than the highest value of 1000w/(m.k) of the product shown in the Panasonic patent with an application number of CN1816504A.
Description
Technical field
the present invention relates to a kind of manufacture method of graphite guide hotting mask.
Background technology
along with the fast development of semiconductor technology, and digital product is as more and more higher in the requirement to portable performance such as mobile phone, panel computer, and this makes relevant manufacturers in the urgent need to improving the utilization ratio of electronic product internal space.But the heat produced in operation is not easily discharged, is easy to run-up and forms high temperature.Obviously, high temperature can reduce the performance of electronics, reliability and work-ing life.Therefore, Current electronic industry proposes more and more higher requirement for the heat sink material as heat control system core component, is passed by heat rapidly in the urgent need to a kind of high-efficiency heat conduction, light material, ensures that electronics normally runs.
traditional heat sink material is the metal of the high heat conduction of copper, silver, aluminium and so on, but along with the raising of electronic devices and components thermal value, cannot meet product needed.And natural stone ink film has higher thermal conductivity, lower density, good stability of material, so be progressively widely used in electron trade.Natural stone ink film is with natural flake graphite or coal-tar pitch for raw material, and after raw material acidifying, heating makes natural graphite interlayer expand, and obtains vermicular texture, then by with matrix material high-temperature and high-pressure conditions under roll, obtain membranaceous graphite flake.As number of patent application 201010240207.8 and 201110002281.0.
but the thermal conductivity of natural stone ink film is generally no more than 400W (M.K)-1, is easy to the shortcomings such as dry linting in addition, so day by day cannot meet the cooling requirements of current portable digital product.As described in Chinese patent application publication number CN1816504A, CN103193221A, be a kind of technique being different from natural stone ink film, adopt with macromolecule membrane or relevant monomer as raw material, obtain synthetic graphite film by nearly 3000 degree of pyroprocessing.
the object of the present invention is to provide a kind of manufacture method of novel artificial synthetic graphite heat conducting film.Involved graphite film, with polyimide (PI) film for main raw material, is positioned in boat, places 3-50 and opens PI film, through carbonization and graphitization processing, prepare the crystallinity foam materials that main component is carbon in every two graphite papers.Again by roll-in or laminating technology, obtain that soft surface is smooth, the uniform high conduction graphite film of thickness.
Summary of the invention
technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of manufacture method of graphite guide hotting mask.
for solving above technical problem, the present invention takes following technical scheme:
a manufacture method for graphite guide hotting mask, is characterized in that: comprise the following steps:
(1) by Kapton through plasma treatment;
(2) between two graphite papers, place 3 ~ 50 Kaptons processed through step (1), carry out hyperthermic treatment and obtain crystalline carbon foam film;
(3) by roll-in or lamination, carbon foam film is processed as ganoid graphite guide hotting mask.
preferably, described step (2) comprising:
(2-1) described graphite paper and Kapton are put into carbide furnace, the air pressure in carbide furnace is controlled at 0.05 ~ 0.5KPa, be warming up to 400 ~ 600 DEG C with per minute 5 ~ 30 DEG C of degree;
(2-2) continue to be warming up to 700 ~ 900 DEG C with per minute 5 ~ 10 DEG C;
(2-2) continue to be warming up to 1000 ~ 1200 DEG C with per minute 2 ~ 8 DEG C, constant temperature half an hour;
(2-3) close carbide furnace, after Temperature fall, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after being vacuumized by graphitizing furnace, passing into rare gas element to interior pressure is 1.05 ~ 1.25atm, and be warming up to 1000 ~ 1200 DEG C with per minute 5-30 DEG C, interior pressure is increased to 1.3 ~ 1.8atm;
(2-5) continue to heat up with per minute 5-15 DEG C, often heat up 200 DEG C, temperature oscillation 5 ~ 30 minutes, amplitude is 15-30 DEG C, until be warming up to 2300 ~ 2500 DEG C, reduces pressure to 1.05 ~ 1.2atm;
(2-6) continue to heat up with per minute 2 ~ 5 DEG C, often heat up 100 DEG C, temperature oscillation 5 ~ 20 minutes, amplitude is 5-20 DEG C.Until be warming up to 2800 ~ 3000 DEG C, constant temperature is after 20 ~ 50 minutes, and Temperature fall, obtains crystalline carbon foam film.
preferably, described step (2) comprising:
(2-1) described graphite paper and Kapton are put into carbide furnace, the air pressure in carbide furnace is controlled at 0.2KPa, be warming up to 500 DEG C with per minute 10 DEG C of degree;
(2-2) continue to be warming up to 800 DEG C with per minute 8 DEG C;
(2-2) continue to be warming up to 1100 DEG C with per minute 6 DEG C, constant temperature half an hour;
(2-3) close carbide furnace, after Temperature fall, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after being vacuumized by graphitizing furnace, passing into rare gas element to interior pressure is 1.2atm, and be warming up to 1100 DEG C with per minute 10 DEG C, interior pressure is increased to 1.4atm;
(2-5) continue to heat up with per minute 6 DEG C, often heat up 200 DEG C, temperature oscillation 20 minutes, amplitude is 20 DEG C, until be warming up to 2400 DEG C, reduces pressure to 1.1atm;
(2-6) continue to heat up with per minute 4 DEG C, often heat up 100 DEG C, temperature oscillation 10 minutes, amplitude is 10 DEG C.Until be warming up to 2900 DEG C, constant temperature is after 30 minutes, and Temperature fall, obtains crystalline carbon foam film.
preferably, the rare gas element passed in step (2-4) is argon gas.
preferably, after described graphite paper and Kapton are loaded boat, boat is put into carbide furnace and graphitizing furnace.
due to the employing of above technical scheme, the present invention compared with prior art tool has the following advantages:
the productivity ratio manufacture method of the prior art of the manufacture method of graphite guide hotting mask of the present invention improves 1-5 doubly, and yield is stablized.Product surface soft smooth, does not have surperficial bad thermal conductivity to be greater than 1800w/ (m.k), higher than PANASONIC number of patent application CN1816504A expressed by maximum 1000 w/ (m.k).By Kapton through plasma treatment, have two kinds of effects: surface cleaning, surface active particularly surface imperfection as pin hole.By plasma treatment, shrinking percentage and some superficial punctate that can reduce graphite film are bad.
Embodiment
below in conjunction with specific embodiment, the present invention is described in further details.Should be understood that these embodiments are for illustration of ultimate principle of the present invention, principal character and advantage, and the present invention does not limit by the scope of following examples.The implementation condition adopted in embodiment can do further adjustment according to specific requirement, and not marked implementation condition is generally the condition in normal experiment.
embodiment 1
by Kapton through plasma treatment, placing graphite paper and Kapton in boat, have the Kapton of 15, boat put into carbide furnace, is evacuated to 0.2KPa, be warming up to 500 DEG C with per minute 10 DEG C in the middle of every two-layer graphite paper; Then be warming up to 800 DEG C with per minute 8 DEG C, be finally warming up to 1100 DEG C with per minute 6 DEG C, constant temperature half an hour.Closing device, takes out boat after Temperature fall to normal temperature, puts into graphitizing furnace.After being vacuumized by graphitizing furnace, passing into straight argon to interior pressure is 1.2atm, is warming up to 1100 DEG C with per minute 10 DEG C, increases pressure to 1.4atm; Then with per minute 6 DEG C intensification, often heat up 200 DEG C can temperature oscillation 20 minutes, amplitude is 20 DEG C.After temperature rises to 2400 DEG C, reduce pressure to 1.1atm, per minute heats up 4 DEG C, every 100 DEG C can temperature oscillation 10 minutes, amplitude is 10 DEG C.After temperature rises to 2900 DEG C, constant temperature shut down after 30 minutes, and Temperature fall obtains crystalline carbon foam film.By roll-in or lamination, carbon foam film is processed as ganoid graphite guide hotting mask.
embodiment 2
by Kapton through plasma treatment, placing graphite paper and Kapton in boat, have the Kapton of 3, boat put into carbide furnace, is evacuated to 0.05KPa, be warming up to 400 DEG C with per minute 5 DEG C in the middle of every two-layer graphite paper; Then be warming up to 700 DEG C with per minute 5 DEG C, be finally warming up to 1000 DEG C with per minute 2 DEG C, constant temperature half an hour.Closing device, takes out boat after Temperature fall to normal temperature, puts into graphitizing furnace.After being vacuumized by graphitizing furnace, passing into straight argon to interior pressure is 1.05atm, is warming up to 1000 DEG C with per minute 5 DEG C, increases pressure to 1.3atm; Then with per minute 5 DEG C intensification, often heat up 200 DEG C can temperature oscillation 5 minutes, amplitude is 15 DEG C.After temperature rises to 2300 DEG C, reduce pressure to 1.05atm, per minute heats up 2 DEG C, every 100 DEG C can temperature oscillation 5 minutes, amplitude is 5 DEG C.After temperature rises to 2800 DEG C, constant temperature shut down after 20 minutes, and Temperature fall obtains crystalline carbon foam film.By roll-in or lamination, carbon foam film is processed as ganoid graphite guide hotting mask.
embodiment 3
by Kapton through plasma treatment, placing graphite paper and Kapton in boat, have the Kapton of 50, boat put into carbide furnace, is evacuated to 0.5KPa, be warming up to 600 DEG C with per minute 30 DEG C in the middle of every two-layer graphite paper; Then be warming up to 900 DEG C with per minute 10 DEG C, be finally warming up to 1200 DEG C with per minute 8 DEG C, constant temperature half an hour.Closing device, takes out boat after Temperature fall to normal temperature, puts into graphitizing furnace.After being vacuumized by graphitizing furnace, passing into straight argon to interior pressure is 1.25atm, is warming up to 1200 DEG C with per minute 30 DEG C, increases pressure to 1.8atm; Then with per minute 15 DEG C intensification, often heat up 200 DEG C can temperature oscillation 20 minutes, amplitude is 20 DEG C.After temperature rises to 3000 DEG C, reduce pressure to 1.2atm, per minute heats up 5 DEG C, every 100 DEG C can temperature oscillation 20 minutes, amplitude is 20 DEG C.After temperature rises to 3000 DEG C, constant temperature shut down after 50 minutes, and Temperature fall obtains crystalline carbon foam film.By roll-in or lamination, carbon foam film is processed as ganoid graphite guide hotting mask.
above to invention has been detailed description; the explanation of embodiment just understands method of the present invention and core concept thereof for helping; its object is to allow the personage being familiar with this art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. a manufacture method for graphite guide hotting mask, is characterized in that: comprise the following steps:
(1) by Kapton through plasma treatment;
(2) between two graphite papers, place 3 ~ 50 Kaptons processed through step (1), carry out hyperthermic treatment and obtain crystalline carbon foam film;
(3) by roll-in or lamination, carbon foam film is processed as ganoid graphite guide hotting mask.
2. the manufacture method of a kind of graphite guide hotting mask according to claim 1, is characterized in that: described step (2) comprising:
(2-1) described graphite paper and Kapton are put into carbide furnace, control at 0.05 ~ 0.5KPa by the air pressure in carbide furnace, the mode raising 5 ~ 30 DEG C with per minute is warming up to 400 ~ 600 DEG C;
(2-2) continue to be warming up to 700 ~ 900 DEG C in the mode of per minute rising 5 ~ 10 DEG C;
(2-2) raise the mode of 2 ~ 8 DEG C with per minute to continue to be warming up to 1000 ~ 1200 DEG C, constant temperature half an hour;
(2-3) close carbide furnace, after Temperature fall, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after being vacuumized by graphitizing furnace, passing into rare gas element to interior pressure is 1.05 ~ 1.25atm, and the mode raising 5-30 DEG C with per minute is warming up to 1000 ~ 1200 DEG C, and interior pressure is increased to 1.3 ~ 1.8atm;
(2-5) continue to heat up in the mode of per minute rising 5-15 DEG C, often heat up 200 DEG C, temperature oscillation 5 ~ 30 minutes, amplitude is 15-30 DEG C, until be warming up to 2300 ~ 2500 DEG C, reduces pressure to 1.05 ~ 1.2atm;
(2-6) continue to heat up in the mode of per minute rising 2 ~ 5 DEG C, often heat up 100 DEG C, temperature oscillation 5 ~ 20 minutes, amplitude is 5-20 DEG C, until be warming up to 2800 ~ 3000 DEG C, constant temperature is after 20 ~ 50 minutes, and Temperature fall, obtains crystalline carbon foam film.
3. the manufacture method of a kind of graphite guide hotting mask according to claim 1, is characterized in that: described step (2) comprising:
(2-1) described graphite paper and Kapton are put into carbide furnace, control at 0.2KPa by the air pressure in carbide furnace, the mode raising 10 DEG C with per minute is warming up to 500 DEG C;
(2-2) mode raising 8 DEG C with per minute continues to be warming up to 800 DEG C;
(2-2) mode raising 6 DEG C with per minute continues to be warming up to 1100 DEG C, constant temperature half an hour;
(2-3) close carbide furnace, after Temperature fall, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after being vacuumized by graphitizing furnace, passing into rare gas element to interior pressure is 1.2atm, and be warming up to 1100 DEG C with per minute 10 DEG C, interior pressure is increased to 1.4atm;
(2-5) continue to heat up with per minute 6 DEG C, often heat up 200 DEG C, temperature oscillation 20 minutes, amplitude is 20 DEG C, until be warming up to 2400 DEG C, reduces pressure to 1.1atm;
(2-6) mode raising 4 DEG C with per minute continues to heat up, and often heat up 100 DEG C, temperature oscillation 10 minutes, amplitude is 10 DEG C, until be warming up to 2900 DEG C, constant temperature is after 30 minutes, and Temperature fall, obtains crystalline carbon foam film.
4. the manufacture method of a kind of graphite guide hotting mask according to claim 2, is characterized in that: the rare gas element passed in step (2-4) is argon gas.
5. the manufacture method of a kind of graphite guide hotting mask according to claim 2, is characterized in that: after described graphite paper and Kapton are loaded boat, boat is put into carbide furnace and graphitizing furnace.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410700634.8A CN104495798B (en) | 2014-11-28 | 2014-11-28 | A kind of manufacture method of graphite guide hotting mask |
| PCT/CN2014/095479 WO2016082280A1 (en) | 2014-11-28 | 2014-12-30 | Method for manufacturing heat-conduction graphite film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410700634.8A CN104495798B (en) | 2014-11-28 | 2014-11-28 | A kind of manufacture method of graphite guide hotting mask |
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| CN104495798A true CN104495798A (en) | 2015-04-08 |
| CN104495798B CN104495798B (en) | 2016-05-11 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105666979A (en) * | 2016-01-13 | 2016-06-15 | 山东安诺克新材料有限公司 | Graphite film with thermal conductivity and preparation method thereof |
| CN106115670A (en) * | 2016-06-23 | 2016-11-16 | 苏州格优碳素新材料有限公司 | A kind of package Delanium heat dissipation film manufacture method |
| CN107090275A (en) * | 2017-05-27 | 2017-08-25 | 杭州高烯科技有限公司 | A kind of graphene/polyimides of high heat conduction is combined carbon film and preparation method thereof |
| CN107162594A (en) * | 2017-05-31 | 2017-09-15 | 杭州高烯科技有限公司 | A kind of polyimide-based compound carbon film of high heat conduction and preparation method thereof |
| US20180244525A1 (en) * | 2017-02-27 | 2018-08-30 | Shenzhen Danbond Technology Co., Ltd | Roll-shaped and continuous graphene film and manufacturing method therefor |
| WO2018153039A1 (en) * | 2017-02-27 | 2018-08-30 | 深圳丹邦科技股份有限公司 | Roll-shaped continuous graphene thin film and preparation method therefor |
| WO2018219000A1 (en) * | 2017-05-27 | 2018-12-06 | 杭州高烯科技有限公司 | Polyimide-based composite carbon film with high thermal conductivity and preparation method therefor |
| CN110092374A (en) * | 2019-05-28 | 2019-08-06 | 宇冠芯龙(武汉)科技有限公司 | A kind of preparation method and graphite film material of electrographite film |
| CN110451964A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | A kind of preparation method of high orientation Graphite block material |
| CN111548161A (en) * | 2020-04-26 | 2020-08-18 | 安徽恒炭新材料科技有限公司 | Method for manufacturing super-thick artificial graphite film |
| CN112897521A (en) * | 2021-01-15 | 2021-06-04 | 王立勇 | Preparation method of graphite film composite material |
| CN113666369A (en) * | 2021-09-10 | 2021-11-19 | 东莞市鸿亿导热材料有限公司 | Alkene carbon film and preparation method thereof |
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| TW201406537A (en) * | 2012-08-09 | 2014-02-16 | Hugetemp Energy Ltd | Material stacking structure of flexible graphite paper and method of producing flexible graphite paper |
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- 2014-12-30 WO PCT/CN2014/095479 patent/WO2016082280A1/en active Application Filing
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| 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 |
| CN103864068A (en) * | 2014-03-26 | 2014-06-18 | 苏州格优碳素新材料有限公司 | Method for preparing graphite film with high heat conductivity |
| CN103922324A (en) * | 2014-04-11 | 2014-07-16 | 江苏悦达新材料科技有限公司 | Preparation method of graphite film with high heat conductivity |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105666979A (en) * | 2016-01-13 | 2016-06-15 | 山东安诺克新材料有限公司 | Graphite film with thermal conductivity and preparation method thereof |
| CN106115670A (en) * | 2016-06-23 | 2016-11-16 | 苏州格优碳素新材料有限公司 | A kind of package Delanium heat dissipation film manufacture method |
| WO2018153039A1 (en) * | 2017-02-27 | 2018-08-30 | 深圳丹邦科技股份有限公司 | Roll-shaped continuous graphene thin film and preparation method therefor |
| US10676362B2 (en) * | 2017-02-27 | 2020-06-09 | Shenzhen Danbond Technology Co., Ltd | Roll-shaped and continuous graphene film and manufacturing method therefor |
| US20180244525A1 (en) * | 2017-02-27 | 2018-08-30 | Shenzhen Danbond Technology Co., Ltd | Roll-shaped and continuous graphene film and manufacturing method therefor |
| WO2018219000A1 (en) * | 2017-05-27 | 2018-12-06 | 杭州高烯科技有限公司 | Polyimide-based composite carbon film with high thermal conductivity and preparation method therefor |
| CN107090275A (en) * | 2017-05-27 | 2017-08-25 | 杭州高烯科技有限公司 | A kind of graphene/polyimides of high heat conduction is combined carbon film and preparation method thereof |
| JP2020521712A (en) * | 2017-05-27 | 2020-07-27 | ハンヂョウ ガオシー テクノロジー カンパニー リミテッドＨａｎｇｚｈｏｕ Ｇａｏｘｉ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｔｄ． | High thermal conductivity polyimide-based composite carbon film and method for producing the same |
| CN107162594A (en) * | 2017-05-31 | 2017-09-15 | 杭州高烯科技有限公司 | A kind of polyimide-based compound carbon film of high heat conduction and preparation method thereof |
| CN110092374A (en) * | 2019-05-28 | 2019-08-06 | 宇冠芯龙(武汉)科技有限公司 | A kind of preparation method and graphite film material of electrographite film |
| CN110451964A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | A kind of preparation method of high orientation Graphite block material |
| CN111548161A (en) * | 2020-04-26 | 2020-08-18 | 安徽恒炭新材料科技有限公司 | Method for manufacturing super-thick artificial graphite film |
| CN112897521A (en) * | 2021-01-15 | 2021-06-04 | 王立勇 | Preparation method of graphite film composite material |
| CN113666369A (en) * | 2021-09-10 | 2021-11-19 | 东莞市鸿亿导热材料有限公司 | Alkene carbon film and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104495798B (en) | 2016-05-11 |
| WO2016082280A1 (en) | 2016-06-02 |
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Address after: Wujiang District of Suzhou city cloud pear road 215217 Jiangsu province No. 657 Patentee after: Jiangsu GeYou carbon new material Co., Ltd Address before: Wujiang District of Suzhou city cloud pear road 215217 Jiangsu province No. 657 Patentee before: SUZHOU YOUGE CARBON NEW MATERIAL CO., LTD. |
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