CN104909358A - Preparation method of large-size high-heat conduction graphite membrane - Google Patents
Preparation method of large-size high-heat conduction graphite membrane Download PDFInfo
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- CN104909358A CN104909358A CN201510269073.5A CN201510269073A CN104909358A CN 104909358 A CN104909358 A CN 104909358A CN 201510269073 A CN201510269073 A CN 201510269073A CN 104909358 A CN104909358 A CN 104909358A
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Abstract
The invention discloses a preparation method of a large-size high-heat conduction graphite membrane. The preparation method comprises the following steps of 1, PI film overlapping, 2, heat treatment carbonization, 3, pressurization and 4, rolling. The large-size high-heat conduction graphite membrane subjected to heat treatment has a graphitization degree of 74.4%, density of 2.12g/cm<3> close to single crystal graphite density of 2.267g/cm<3>, heat conductivity of 850W/(m.K)-1000W/(m.K) and a product thickness tolerance scope within +/- 2 micrometers.
Description
Technical field
The present invention relates to a kind of preparation method of large size high conduction graphite film, be suitable for circuit card and the chip of various electronic product.
Background technology
High starch breeding has excellent electrical and thermal conductivity performance, is the indispensable ideal material of modern development in science and technology.Shanxi coalification institute of Chinese Academy of Sciences Zhai waits more very much that people utilizes PI pellicular cascade, heat pressing process develops the high conductive graphite block materials that thermal conductivity is greater than 600W/ (mK).Organic polymer charing black lead treating processes pyrolytic reaction complicated mechanism, for easy greying raw material, charing process is also little for the impact of sample microlitic structure, and what really make microtexture generation qualitative change is in the greying stage
h(HTT>2000 ° of C).Although many researchists have done a lot of work in this respect, but because of the restriction of research means and test condition, also do not reach completely clearly stage at present.
The large size of current synthetic, ultra-thin, high conduction graphite film, be mainly used in the electronics of limited space, and battery, wireless base station etc. as the high-power die of mobile phone, PAD etc., various electronic product need the environment of cooling.On information products heat radiation market, the production of high-end graphite height heat conducting film is primarily of transnational company's monopolizations such as Panasonics; Domestic graphite height heat conducting film, due to the reason such as performance, quality, can only capture primary market, even embarrasses client to provide the A level graphite height heat conducting film product of whole.
Summary of the invention
For above situation, the object of the present invention is to provide a kind of preparation method of large size high conduction graphite film, that product adopts the research of skeleton structure, starting material and controls, special-purpose catalyst, high/low temperature process, product application research and innovates, can the large size of whole of volume production, surfacing, complete series thickness, excellent heat conducting performance height lead graphite film.It is blank that project implementation will fill up the high graphite film product of leading of domestic large size, break through the technical monopoly of transnational company's high performance graphite film, promote the optimization of the domestic electronic information material industrial structure, drive the downstream electronic information industry development.Making it when reaching the performance of existing product, good end-use performance can also be had.
Technical scheme of the present invention is achieved in the following ways: a kind of preparation method of large size high conduction graphite film, comprises the following steps: 1) PI pellicular cascade, 2) heat treatment carbonization, 3) pressurization, 4) rolling; It is characterized in that:
1), PI pellicular cascade: be put into charring furnace after PI film 80 layer laminate of 40mm by diameter, drift add different weight to produce different pressure;
2), heat treatment carbonization: be tamping charring furnace, open gas cylinder and reducing valve, the flow controlling argon gas is 10mL/min, logical 40min argon gas, guarantees that air is all caught up with to the greatest extent, starts to heat up; Time variable control, after the stage rises to temperature required (500 DEG C, 700 DEG C, 800 DEG C), each constant temperature of thermal treatment temp point one hour;
Described is provided with magnetic induction loop in charring furnace, and magneticstrength is 40-50MT, step 2) heat treated while, magnetic induction loop applies magnetic field to PI film;
3), pressurization: the PI pellicular cascade after charing is carried out the high temperature graphitization process from 2500 DEG C to 2800 DEG C in thermocompressor, mechanical pressurization 200kg/cm
2;
4), rolling: the PI pellicular cascade after charing pressurization is formed large size high conduction graphite film, and rolling is put in storage.
The present invention, large size high conduction graphite film degree of graphitization after heat treatment reaches 74.4%, and density reaches 2.12g/cm
3, close to the density 2.267g/cm of single crystal graphite
3, thermal conductivity is 850W/ (mK) ~ 1000W/ (mK), and product thickness tolerance zone is within ± 2 μm.
Embodiment
A preparation method for large size high conduction graphite film, comprises the following steps:
1, PI pellicular cascade: be put into charring furnace after PI film 80 layer laminate of 40mm by diameter, drift add different weight to produce different pressure;
2, heat treatment carbonization: be tamping charring furnace, opens gas cylinder and reducing valve, and the flow controlling argon gas is 10mL/min, logical 40min argon gas, guarantees that air is all caught up with to the greatest extent, starts to heat up; Time variable control, after the stage rises to temperature required (500 DEG C, 700 DEG C, 800 DEG C), each constant temperature of thermal treatment temp point one hour; In charring furnace, be provided with magnetic induction loop, magneticstrength is 40-50MT, and heat treated while, magnetic induction loop applies magnetic field to PI film;
3, pressurize: the PI pellicular cascade after charing is carried out the high temperature graphitization process from 2500 DEG C to 2800 DEG C in thermocompressor, mechanical pressurization 200kg/cm
2;
4, rolling: the PI pellicular cascade after charing pressurization is formed large size high conduction graphite film, and rolling is put in storage.
The present invention, in the process preparing high starch breeding material, because raw materials used PI film and Kapton are containing heteroatomss such as aerobic, nitrogen, hydrogen, the carbonization process of film is that these heteroatomss depart from, expand the conjugated system forming aromatic molecule, carry out the process of densification; Specifically along with the rising of thermal treatment temp, a large amount of small molecules is as CO, CO2, N
2effusion, in U product, carbon content increases sharply, final remaining based on the charcoal skeleton of galvanized hexagonal wire mesh aspect, XRD spectra shows as the sharpening of diffraction peak and reducing of interfloor distance, time near 2200 DEG C, get rid of the element beyond charcoal completely, the growth of lamination structure, prosperity, charcoal body is to graphite crystal future development.
Claims (2)
1. a preparation method for large size high conduction graphite film, comprises the following steps: 1) PI pellicular cascade, 2) heat treatment carbonization, 3) pressurization, 4) rolling; It is characterized in that:
1), PI pellicular cascade: be put into charring furnace after PI film 80 layer laminate of 40mm by diameter, drift add different weight to produce different pressure;
2), heat treatment carbonization: be tamping charring furnace, open gas cylinder and reducing valve, the flow controlling argon gas is 10mL/min, logical 40min argon gas, guarantees that air is all caught up with to the greatest extent, starts to heat up; Time variable control, after the stage rises to temperature required (500 DEG C, 700 DEG C, 800 DEG C), each constant temperature of thermal treatment temp point one hour;
3), pressurization: the PI pellicular cascade after charing is carried out the high temperature graphitization process from 2500 DEG C to 2800 DEG C in thermocompressor, mechanical pressurization 200kg/cm
2;
4), rolling: the PI pellicular cascade after charing pressurization is formed large size high conduction graphite film, and rolling is put in storage.
2. the preparation method of a kind of large size high conduction graphite film according to claim 1, it is characterized in that: described step 2) in be provided with magnetic induction loop in charring furnace, magneticstrength is 40-50MT, and heat treated while, magnetic induction loop applies magnetic field to PI film.
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| CN201510269073.5A CN104909358A (en) | 2015-05-25 | 2015-05-25 | Preparation method of large-size high-heat conduction graphite membrane |
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| CN201510269073.5A CN104909358A (en) | 2015-05-25 | 2015-05-25 | Preparation method of large-size high-heat conduction graphite membrane |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| CN105752959A (en) * | 2016-03-04 | 2016-07-13 | 深圳丹邦科技股份有限公司 | Thermoplastic polyimide film carbonization composite film and preparation method thereof |
| CN106495147A (en) * | 2016-11-08 | 2017-03-15 | 株洲时代新材料科技股份有限公司 | A kind of method that catalyzed graphitization prepares high heat conduction graphite |
| CN106832926A (en) * | 2017-01-19 | 2017-06-13 | 祝巧凤 | Graphite mixture, graphite film for heat conduction and its preparation method and application |
| WO2021082373A1 (en) * | 2019-10-30 | 2021-05-06 | 深圳丹邦科技股份有限公司 | Compound semiconductor flexible carbon-based film and preparation method therefor |
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| CN103193221A (en) * | 2007-05-17 | 2013-07-10 | 株式会社钟化 | Graphite film and manufacturing method thereof |
| CN104176733A (en) * | 2014-08-25 | 2014-12-03 | 上海弘枫实业有限公司 | Manufacturing method of high-thermal-conductivity graphite film |
| CN104495795A (en) * | 2014-11-24 | 2015-04-08 | 云南云天化股份有限公司 | Graphite flake and preparation method thereof |
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2015
- 2015-05-25 CN CN201510269073.5A patent/CN104909358A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN103193221A (en) * | 2007-05-17 | 2013-07-10 | 株式会社钟化 | Graphite film and manufacturing method thereof |
| CN104176733A (en) * | 2014-08-25 | 2014-12-03 | 上海弘枫实业有限公司 | Manufacturing method of high-thermal-conductivity graphite film |
| CN104495795A (en) * | 2014-11-24 | 2015-04-08 | 云南云天化股份有限公司 | Graphite flake and preparation method thereof |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| CN105752959A (en) * | 2016-03-04 | 2016-07-13 | 深圳丹邦科技股份有限公司 | Thermoplastic polyimide film carbonization composite film and preparation method thereof |
| WO2017148105A1 (en) * | 2016-03-04 | 2017-09-08 | 深圳丹邦科技股份有限公司 | Carbonized membrane prepared from flexible polyimide and preparation method therefor |
| WO2017148106A1 (en) * | 2016-03-04 | 2017-09-08 | 深圳丹邦科技股份有限公司 | Thermoplastic polyimide thin-film carbonized composite membrane, and preparation method therefor |
| CN105600782B (en) * | 2016-03-04 | 2018-06-26 | 深圳丹邦科技股份有限公司 | Carbon film prepared by flexible polyimide and preparation method thereof |
| US11001739B2 (en) | 2016-03-04 | 2021-05-11 | Shenzhen Danbond Technology Co., Ltd | Carbonized composite thermoplastic polyimide film and preparation method thereof |
| US11078081B2 (en) | 2016-03-04 | 2021-08-03 | Shenzhen Danbond Technology Co., Ltd | Graphene film prepared with flexible polyimide and preparation method thereof |
| CN106495147A (en) * | 2016-11-08 | 2017-03-15 | 株洲时代新材料科技股份有限公司 | A kind of method that catalyzed graphitization prepares high heat conduction graphite |
| CN106495147B (en) * | 2016-11-08 | 2018-07-31 | 株洲时代新材料科技股份有限公司 | A kind of method that catalyzed graphitization prepares high heat conduction graphite |
| CN106832926A (en) * | 2017-01-19 | 2017-06-13 | 祝巧凤 | Graphite mixture, graphite film for heat conduction and its preparation method and application |
| CN106832926B (en) * | 2017-01-19 | 2020-03-10 | 祝巧凤 | Graphite mixture for heat conduction, graphite film, and preparation method and application thereof |
| WO2021082373A1 (en) * | 2019-10-30 | 2021-05-06 | 深圳丹邦科技股份有限公司 | Compound semiconductor flexible carbon-based film and preparation method therefor |
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Application publication date: 20150916 |