CN104495798B - A kind of manufacture method of graphite guide hotting mask - Google Patents
A kind of manufacture method of graphite guide hotting mask Download PDFInfo
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- CN104495798B CN104495798B CN201410700634.8A CN201410700634A CN104495798B CN 104495798 B CN104495798 B CN 104495798B CN 201410700634 A CN201410700634 A CN 201410700634A CN 104495798 B CN104495798 B CN 104495798B
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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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- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
<b>The manufacture method that the present invention relates to a kind of graphite guide hotting mask, is characterized in that: comprise the following steps: (</b><b>1</b><b>) by Kapton process plasma treatment; (</b><b>2</b><b>) between two graphite papers, place</b><b>3 ~ 50</b><b>Through step (</b><b>1</b><b>) Kapton processed, carry out hyperthermic treatment and obtain crystalline carbon foam film; (</b><b>3</b><b>) by roll-in or lamination, carbon foam film is processed as to ganoid graphite guide hotting mask. The productivity ratio manufacture method of the prior art of the manufacture method of graphite guide hotting mask of the present invention improves</b><b>1-5</b><b>Times, and yield is stable. Product surface soft smooth, does not have surperficial bad thermal conductivity factor to be greater than</b><b>1800w/ (m.k)</b><b>, higher than the number of patent application of PANASONIC</b><b>CN1816504A</b><b>Expressed peak</b><b>1000? w/ (m.k)</b><b>.</b>
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 to the requirement of portable performance in mobile phone, panel computer etc., and this makes relevant producer in the urgent need to improving the utilization rate of electronic product inner space. But in service produced heat is difficult for discharging, be easy to run-up and form high temperature. Obviously, high temperature can reduce performance, reliability and the service life of electronic equipment. Therefore, current electron trade proposes more and more higher requirement for the heat sink material as heat control system core component, rapidly heat is passed in the urgent need to a kind of high-efficiency heat conduction, light material, ensures that electronic equipment normally moves.
Traditional heat sink material is the metal of the high heat conduction of copper, silver, aluminium and so on, still, along with the raising of electronic devices and components caloric 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 taking natural flake graphite or coal tar pitch as raw material, and by after raw material acidifying, heating is expanded native graphite interlayer, obtains vermicular texture, then by with binding 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 factor of natural stone ink film is generally no more than 400W (M.K)-1, is easy in addition the shortcomings such as dry linting, so day by day cannot meet the heat radiation requirement of current portable digital product. As described in Chinese patent application publication number CN1816504A, CN103193221A, be a kind of technique that is different from natural stone ink film, adopt taking macromolecule membrane or relevant monomer as raw material, obtain artificial-synthetic stone's ink film by nearly 3000 degree high-temperature process.
The object of the present invention is to provide a kind of manufacture method with novel artificial synthetic graphite heat conducting film. Involved graphite film, taking polyimides (PI) film as primary raw material, is positioned in boat, places 3-50 and open PI film in every two graphite papers, and through carbonization and graphitization processing, preparing main component is the crystallinity foamed material of carbon. Again by roll-in or laminating technology, obtain that soft surface is smooth, the high conductive graphite film of even thickness.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of manufacture method of graphite guide hotting mask is provided.
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 process plasma treatment;
(2) between two graphite papers, place 3 ~ 50 Kaptons of processing 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 to 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 to 0.05 ~ 0.5KPa, be warming up to 400 ~ 600 DEG C with 5 ~ 30 DEG C of degree per minute;
(2-2) continue to be warming up to 700 ~ 900 DEG C with 5 ~ 10 DEG C per minute;
(2-2) continue to be warming up to 1000 ~ 1200 DEG C with 2 ~ 8 DEG C per minute, constant temperature half an hour;
(2-3) close carbide furnace, naturally, after cooling, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after graphitizing furnace is vacuumized, passing into inert gas to interior pressure is 1.05 ~ 1.25atm, is warming up to 1000 ~ 1200 DEG C with 5-30 per minute DEG C, and interior pressure is increased to 1.3 ~ 1.8atm;
(2-5) continue to heat up with 5-15 per minute DEG C, 200 DEG C of every intensifications, 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 2 ~ 5 DEG C per minute, 100 DEG C of every intensifications, 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 cooling, obtains crystalline carbon foam film naturally.
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 to 0.2KPa, be warming up to 500 DEG C with 10 DEG C of degree per minute;
(2-2) continue to be warming up to 800 DEG C with 8 DEG C per minute;
(2-2) continue to be warming up to 1100 DEG C with 6 DEG C per minute, constant temperature half an hour;
(2-3) close carbide furnace, naturally, after cooling, take out graphite paper and Kapton;
(2-4) graphite paper and Kapton are put into graphitizing furnace, after graphitizing furnace is vacuumized, passing into inert gas to interior pressure is 1.2atm, is warming up to 1100 DEG C with 10 DEG C per minute, and interior pressure is increased to 1.4atm;
(2-5) continue to heat up with 6 DEG C per minute, 200 DEG C of every intensifications, 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 4 DEG C per minute, 100 DEG C of every intensifications, temperature oscillation 10 minutes, amplitude is 10 DEG C. Until be warming up to 2900 DEG C, constant temperature is after 30 minutes, and cooling, obtains crystalline carbon foam film naturally.
Preferably, the inert gas passing in step (2-4) is argon gas.
Preferably, described graphite paper and Kapton are packed into after 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 stable. Product surface soft smooth, does not have surperficial bad thermal conductivity factor to be greater than 1800w/ (m.k), higher than the expressed peak 1000w/ of number of patent application CN1816504A (m.k) of PANASONIC. Kapton through plasma treatment, is had to two kinds of effects: surface cleaning, surface active particularly blemish as pin hole. By plasma treatment, shrinkage factor and some surperficial point-like that can reduce graphite film are bad.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further details. Should be understood that these embodiment are for general principle of the present invention, principal character and advantage are described, and the present invention is not limited by the scope of following examples. The implementation condition adopting in embodiment can be done 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 in the middle of every two-layer graphite paper, and boat is put into carbide furnace, is evacuated to 0.2KPa, is warming up to 500 DEG C with 10 DEG C per minute; Then be warming up to 800 DEG C with 8 DEG C per minute, be finally warming up to 1100 DEG C with 6 DEG C per minute, constant temperature half an hour. Closing device, takes out boat after being naturally cooled to normal temperature, puts into graphitizing furnace. After graphitizing furnace is vacuumized, passing into straight argon to interior pressure is 1.2atm, is warming up to 1100 DEG C with 10 DEG C per minute, increases pressure to 1.4atm; Then with 6 DEG C of intensifications per minute, 200 DEG C of every intensifications can temperature oscillation 20 minutes, and amplitude is 20 DEG C. Temperature rises to after 2400 DEG C, reduces pressure to 1.1atm, 4 DEG C of intensifications per minute, every 100 DEG C can temperature oscillation 10 minutes, amplitude is 10 DEG C. Temperature rises to after 2900 DEG C, and constant temperature shut down after 30 minutes, and cooling obtains crystalline carbon foam film naturally. By roll-in or lamination, carbon foam film is processed as to ganoid graphite guide hotting mask.
Embodiment 2
By Kapton, through plasma treatment, placing graphite paper and Kapton in boat, have the Kapton of 3 in the middle of every two-layer graphite paper, and boat is put into carbide furnace, is evacuated to 0.05KPa, is warming up to 400 DEG C with 5 DEG C per minute; Then be warming up to 700 DEG C with 5 DEG C per minute, be finally warming up to 1000 DEG C with 2 DEG C per minute, constant temperature half an hour. Closing device, takes out boat after being naturally cooled to normal temperature, puts into graphitizing furnace. After graphitizing furnace is vacuumized, passing into straight argon to interior pressure is 1.05atm, is warming up to 1000 DEG C with 5 DEG C per minute, increases pressure to 1.3atm; Then with 5 DEG C of intensifications per minute, 200 DEG C of every intensifications can temperature oscillation 5 minutes, and amplitude is 15 DEG C. Temperature rises to after 2300 DEG C, reduces pressure to 1.05atm, 2 DEG C of intensifications per minute, every 100 DEG C can temperature oscillation 5 minutes, amplitude is 5 DEG C. Temperature rises to after 2800 DEG C, and constant temperature shut down after 20 minutes, and cooling obtains crystalline carbon foam film naturally. By roll-in or lamination, carbon foam film is processed as to ganoid graphite guide hotting mask.
Embodiment 3
By Kapton, through plasma treatment, placing graphite paper and Kapton in boat, have the Kapton of 50 in the middle of every two-layer graphite paper, and boat is put into carbide furnace, is evacuated to 0.5KPa, is warming up to 600 DEG C with 30 DEG C per minute; Then be warming up to 900 DEG C with 10 DEG C per minute, be finally warming up to 1200 DEG C with 8 DEG C per minute, constant temperature half an hour. Closing device, takes out boat after being naturally cooled to normal temperature, puts into graphitizing furnace. After graphitizing furnace is vacuumized, passing into straight argon to interior pressure is 1.25atm, is warming up to 1200 DEG C with 30 DEG C per minute, increases pressure to 1.8atm; Then with 15 DEG C of intensifications per minute, 200 DEG C of every intensifications can temperature oscillation 20 minutes, and amplitude is 20 DEG C. Temperature rises to after 3000 DEG C, reduces pressure to 1.2atm, 5 DEG C of intensifications per minute, every 100 DEG C can temperature oscillation 20 minutes, amplitude is 20 DEG C. Temperature rises to after 3000 DEG C, and constant temperature shut down after 50 minutes, and cooling obtains crystalline carbon foam film naturally. By roll-in or lamination, carbon foam film is processed as to ganoid graphite guide hotting mask.
Above the present invention is described in detail; the explanation of embodiment is just for helping to understand method of the present invention and core concept thereof; its object is to allow the personage who is 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 that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (4)
1. a manufacture method for graphite guide hotting mask, is characterized in that: comprise the following steps:
(1) by Kapton process plasma treatment;
(2) between two graphite papers, place 3 ~ 50 Kaptons of processing 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 to ganoid graphite guide hotting mask,
It is characterized in that: 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, is warming up to 400 ~ 600 DEG C in the mode of 5 ~ 30 DEG C of risings per minute;
(2-2) continue to be warming up to 700 ~ 900 DEG C in the mode of 5 ~ 10 DEG C of risings per minute;
(2-3) continue to be warming up to 1000 ~ 1200 DEG C in the mode of 2 ~ 8 DEG C of risings per minute, constant temperature half an hour;
(2-4) close carbide furnace, naturally, after cooling, take out graphite paper and Kapton;
(2-5) graphite paper and Kapton are put into graphitizing furnace, after graphitizing furnace is vacuumized, passing into inert gas to interior pressure is 1.05 ~ 1.25atm, is warming up to 1000 ~ 1200 DEG C in the mode of rising 5-30 per minute DEG C, and interior pressure is increased to 1.3 ~ 1.8atm;
(2-6) continue to heat up in the mode of rising 5-15 per minute DEG C, 200 DEG C of every intensifications, 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;
(2-7) continue to heat up in the mode of 2 ~ 5 DEG C of risings per minute, 100 DEG C of every intensifications, 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, cooling, obtains crystalline carbon foam film naturally.
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, the air pressure in carbide furnace is controlled to 0.2KPa, be warming up to 500 DEG C in the mode of 10 DEG C of risings per minute;
(2-2) continue to be warming up to 800 DEG C in the mode of 8 DEG C of risings per minute;
(2-3) continue to be warming up to 1100 DEG C in the mode of 6 DEG C of risings per minute, constant temperature half an hour;
(2-4) close carbide furnace, naturally, after cooling, take out graphite paper and Kapton;
(2-5) graphite paper and Kapton are put into graphitizing furnace, after graphitizing furnace is vacuumized, passing into inert gas to interior pressure is 1.2atm, is warming up to 1100 DEG C with 10 DEG C per minute, and interior pressure is increased to 1.4atm;
(2-6) continue to heat up with 6 DEG C per minute, 200 DEG C of every intensifications, temperature oscillation 20 minutes, amplitude is 20 DEG C, until be warming up to 2400 DEG C, reduces pressure to 1.1atm;
(2-7) continue to heat up in the mode of 4 DEG C of risings per minute, 100 DEG C of every intensifications, temperature oscillation 10 minutes, amplitude is 10 DEG C, until be warming up to 2900 DEG C, constant temperature is after 30 minutes, cooling, obtains crystalline carbon foam film naturally.
3. the manufacture method of a kind of graphite guide hotting mask according to claim 1, is characterized in that: the inert gas passing in step (2-5) is argon gas.
4. the manufacture method of a kind of graphite guide hotting mask according to claim 1, is characterized in that: described graphite paper and Kapton are packed into after boat, boat is put into carbide furnace and graphitizing furnace.
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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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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 |
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US10676362B2 (en) * | 2017-02-27 | 2020-06-09 | Shenzhen Danbond Technology Co., Ltd | Roll-shaped and continuous graphene film and manufacturing method therefor |
US11535567B2 (en) * | 2017-05-27 | 2022-12-27 | Hangzhou Gaoxi Technology Co., Ltd. | Polyimide-based composite carbon film with high thermal conductivity and preparation method therefor |
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 |
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 |
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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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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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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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 |
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