CN103906416A - Method for manufacturing artificial graphite radiating film with catalytic graphitization technology - Google Patents
Method for manufacturing artificial graphite radiating film with catalytic graphitization technology Download PDFInfo
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- CN103906416A CN103906416A CN201410144331.2A CN201410144331A CN103906416A CN 103906416 A CN103906416 A CN 103906416A CN 201410144331 A CN201410144331 A CN 201410144331A CN 103906416 A CN103906416 A CN 103906416A
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Abstract
The invention discloses a method for manufacturing new macromolecule materials, and particularly relates to a method for manufacturing an artificial graphite radiating film with the catalytic graphitization technology. Macromolecule thin films are adopted for serving as raw materials, catalysts are arranged on the surfaces of the macromolecule thin films through spraying, chemical vapor deposition or electrolytic deposition, and graphite paper is clamped between the macromolecule thin films. After the macromolecule thin films separated by the graphite paper are stacked in an intersected mode, the artificial high-thermal-conductivity graphite radiating film is obtained through the carbonization and graphitization processes. Due to the effect of the catalysts, the graphitization temperature can be greatly reduced, the graphitization time can be shortened, energy saving and consumption reducing can be achieved, the production and manufacturing cost can be reduced, and the method is of great significance on large-scale production.
Description
Technical field
The present invention relates to a kind of preparation technology of high heat conduction new material, particularly a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film.
Technical background
Along with the high speed development of microelectronics industry, electronic product, LED etc. are constantly to high-power future development, and integrated circuit high speed, densification increasingly, there will be increasing heating problem, and product power is reduced, and the lost of life, reduces its reliability.
At present, various heat sink materials are widely used.For example metal material has good heat conductivility, as copper, aluminium etc., utilizes these metal radiators to be widely used.But weight metal is large, not corrosion-resistant, and after there is oxidation, its heat dispersion can reduce greatly.Meanwhile, there is in recent years the miniaturization of the various device of the heater members such as semiconductor element mounted thereon, and the tendency of the caloric value of these parts increase, use metal to be restricted as the space of the parts of heat sink material.
Electrographite film is that to form in layer structure, its face thermal conductivity by carbon very high, and density gently arrives 1.0-2.0g/cm
3left and right, can spread rapidly heat that heating position produces to reduce device temperature, also has the feature of flexibility as film, is therefore expected to heat transfer device material or radiator material as narrow place or the place that need to process through gap always.At present, the preparation process of electrographite film mainly contains carbonization and two technical processs of graphitization.But the heat treatment temperature required due to preparation is higher, especially graphitizing process, corresponding high temperature energy consumption is large, the high-temperature service life-span, short its production cost that caused was higher, and people have studied multiple improving one's methods for this reason, as optimized graphitizing furnace structure, graphite heater oxidation resistant coating, select optimum temperature rise, rate of temperature fall and warp tension ratio, improve graphitization atmosphere, in original inert atmosphere (argon gas, nitrogen), add CCl
4, prevent from generating metal carbides, nitride, to extend graphitizing furnace tube lifetime etc., but effective method still adopts catalyst to carry out catalyzed graphitization to reduce graphited temperature, extends the useful life of graphitizing furnace.
Summary of the invention
The object of the invention is, overcome the deficiencies in the prior art, a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film is provided.
Technical solution of the present invention is that employing macromolecule membrane, as raw material, at macromolecule membrane surface spraying, chemical vapour deposition (CVD) or electro-deposition catalyst, then sandwiches graphite paper between macromolecule membrane; Obtain artificial high conductive graphite heat dissipation film through carbonization, graphitizing process again by being separated with the macromolecule membrane of graphite paper after cross layered.Concrete step of preparation process is as follows:
(1) select high molecular film material as raw material, macromolecule membrane surface spraying, chemical vapour deposition (CVD) or electro-deposition catalyst, between the macromolecule membrane of a stator number, compartment inserts graphite paper, intersects stackingly, is finally positioned in graphite boat;
(2) carbide furnace is first evacuated in 5～10Pa, then the graphite boat that fills raw material is put into carbide furnace is warming up to carburizing temperature in the regular hour, carry out carbonization;
(3) material complete carbonization is moved to and in graphitizing furnace, within the regular hour, be warming up to graphitization temperature, and material is applied to certain ambient pressure, graphitization is carried out in inert atmosphere.
The one of wherein said high molecular film material Wei polyoxadiazole, polyimides, polyphenylene vinylene, polybenzimidazoles, polybenzoxazole, polythiazole or polyamide, and then preferred polyimides, its thickness is 15 μ m～100 μ m.
The thickness of described graphite paper is 2～5mm.
Described macromolecule membrane laminates number is generally good within the scope of 1～60.
Described catalyst is one or more mixtures in boric acid, boron nitride, boron carbide, carborundum, iron oxide, calcium carbonate, copper chloride; The addition of catalyst is 0.1-3%, and preferred value is 0.5-1.5%.
Described carbonization time, at 2～10h, and then is preferably 5h.
Described carburizing temperature, at 800～1200 DEG C, and then is preferably 1000 DEG C.
Described graphitization time, at 2～12h, and then is preferably 8h.
Described graphitization temperature, at 2000-2800 DEG C DEG C, and then is preferably 2400 DEG C.
The ambient pressure applying when described graphitization, generally at 10～50g/cm
2interior is good.
Described inert atmosphere is argon gas, nitrogen or helium one or more mixtures in both.
Compared with prior art, the advantage possessing is that process is simple, adds catalyst can greatly reduce graphited temperature, shortens graphitization time, can significantly reduce the impact of pyroprocess on the graphitizing furnace life-span, reduces production costs in the present invention; The ambient pressure simultaneously film being applied when graphitization contributes to eliminate fold and the other defect of heat conducting film, in ensureing high-cooling property, its bubble degree and bubble-domain size are good, and resistance to bend(ing) can be excellent, have met the thin and light demand of the products such as electronic apparatus.
Embodiment
Embodiment 1
Taking polyimides as raw material film, thickness is 35 μ m, at polyimide film surface spraying boron nitride, addition is 0.5%, graphite paper thickness is 3mm, polyimide film and graphite paper is cut into certain specification for subsequent use, puts into 5 polyimides raw material films between two graphite papers, intersect stackingly, be finally positioned in graphite boat.Carbide furnace is evacuated in 5～10Pa, the graphite boat that fills raw material film is put into carbide furnace and carry out carbonization, and carburizing temperature is 1000 DEG C, and the time is 6h, then the material after carbonization is moved in graphitizing furnace, and material is applied to 20 g/cm
2pressure, graphitization temperature is 2400 DEG C, time 7h, graphitizing process carries out under nitrogen atmosphere.The conductive coefficient that finally obtains electrographite heat dissipation film through measuring is 1600 W/mK, does not break through 20000 bendings.
Embodiment 2
Taking polybenzoxazole as raw material film, thickness is 50 μ m, at polybenzoxazole film surface chemistry vapour deposition iron oxide, addition is 1.5%, graphite paper thickness is 4mm, polybenzoxazole thin film and graphite paper is cut into certain specification for subsequent use, puts into 20 polybenzoxazole raw material films between two graphite papers, intersect stackingly, be finally positioned in graphite boat.Carbide furnace is evacuated in 5～10Pa, the graphite boat that fills raw material film is put into carbide furnace and carry out carbonization, and carburizing temperature is 900 DEG C, and the time is 8h, then the material after carbonization is moved in graphitizing furnace, and material is applied to 30 g/cm
2pressure, graphitization temperature is 2200 DEG C, time 8h, graphitizing process carries out under argon gas atmosphere.The conductive coefficient that finally obtains electrographite heat dissipation film through measuring is 1800 W/mK, does not break through 20000 bendings.
Embodiment 3
Taking polyamide as raw material film, thickness is 25 μ m, at polyamide surface electro-deposition copper chloride, addition is 3%, graphite paper thickness is 5mm, polyamide film and graphite paper is cut into certain specification for subsequent use, puts into 40 polyamide raw materials films between two graphite papers, intersect stackingly, be finally positioned in graphite boat.Carbide furnace is evacuated in 5～10Pa, the graphite boat that fills raw material film is put into carbide furnace and carry out carbonization, and carburizing temperature is 1000 DEG C, and the time is 5h, then the material after carbonization is moved in graphitizing furnace, and material is applied to 10 g/cm
2pressure, graphitization temperature is 2600 DEG C, time 9h, graphitizing process carries out under helium atmosphere.The conductive coefficient that finally obtains electrographite heat dissipation film through measuring is 1750 W/mK, does not break through 20000 bendings.
Claims (6)
1. a method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film, it is characterized in that: adopt macromolecule membrane as raw material, at macromolecule membrane surface spraying, chemical vapour deposition (CVD) or electro-deposition catalyst, then between macromolecule membrane, sandwich graphite paper; Obtain electrographite heat dissipation film through carbonization, graphitization technique again by being separated with the macromolecule membrane of graphite paper after cross layered.
2. a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film according to claim 1, is characterized in that: described macromolecule membrane is the one in polyoxadiazole, polyimides, polyphenylene vinylene, polybenzimidazoles, polybenzoxazole, polythiazole or polyamide; Its thickness is 15 μ m～100 μ m.
3. a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film according to claim 1, is characterized in that: the thickness of graphite paper is 2～5mm, macromolecule membrane lamination number is 1～60.
4. a kind of method of utilizing catalytic graphite metallization processes to prepare artificial heat dissipation film according to claim 1, is characterized in that: catalyst is one or more mixtures in boric acid, boron nitride, boron carbide, carborundum, iron oxide, calcium carbonate, copper chloride; The addition of catalyst is 0.1-3%, and preferred value is 0.5-1.5%.
5. a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film according to claim 1, is characterized in that: when carbonization, temperature is 800-1200 DEG C, the time is 2～10h, and preferably temperature and time is respectively 1000 DEG C and 5h; Carbonization is carried out under vacuum environment, and vacuum is in 5～10Pa.
6. a kind of method of utilizing catalytic graphite metallization processes to prepare electrographite heat dissipation film according to claim 1, is characterized in that: graphitization temperature is 2000-2800 DEG C, the time is 2-12h, and preferably temperature and time is respectively 2400 DEG C and 8h; Graphitization is carried out under inert atmosphere, and inert atmosphere is one or several mixture in nitrogen, argon gas or helium, and the ambient pressure applying when graphitization is 10～50g/cm
2.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104329855A (en) * | 2014-08-29 | 2015-02-04 | 青岛海尔股份有限公司 | Semiconductor refrigeration refrigerator and manufacturing method thereof |
| CN104853519A (en) * | 2015-05-26 | 2015-08-19 | 江苏悦达新材料科技有限公司 | Flexible conducting circuit and manufacturing method thereof |
| CN106083051A (en) * | 2016-06-15 | 2016-11-09 | 黄志良 | High conductive graphite heat dissipation film processing technology |
| CN106832923A (en) * | 2016-12-16 | 2017-06-13 | 深圳瑞华泰薄膜科技有限公司 | A kind of Kapton for preparing electrographite 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 |
| CN112552681A (en) * | 2020-12-07 | 2021-03-26 | 上海电力大学 | Functionalized boron nitride nanosheet/MXene/polybenzimidazole high-thermal-conductivity composite film and preparation method thereof |
| US11502304B2 (en) * | 2019-11-08 | 2022-11-15 | Enevate Corporation | Catalysts and methods for lowering electrode pyrolysis temperature |
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| CN106083051A (en) * | 2016-06-15 | 2016-11-09 | 黄志良 | High conductive graphite heat dissipation film processing technology |
| CN106832923A (en) * | 2016-12-16 | 2017-06-13 | 深圳瑞华泰薄膜科技有限公司 | A kind of Kapton for preparing electrographite film and preparation method thereof |
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| 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 |
| US11502304B2 (en) * | 2019-11-08 | 2022-11-15 | Enevate Corporation | Catalysts and methods for lowering electrode pyrolysis temperature |
| EP4055652A4 (en) * | 2019-11-08 | 2023-12-06 | Enevate Corporation | Catalysts and methods for lowering electrode pyrolysis temperature |
| CN112552681A (en) * | 2020-12-07 | 2021-03-26 | 上海电力大学 | Functionalized boron nitride nanosheet/MXene/polybenzimidazole high-thermal-conductivity composite film and preparation method thereof |
| CN112552681B (en) * | 2020-12-07 | 2022-08-05 | 上海电力大学 | Functionalized boron nitride nanosheet/MXene/polybenzimidazole high-thermal-conductivity composite film and preparation method thereof |
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Application publication date: 20140702 |