CN104176733A - Manufacturing method of high-thermal-conductivity graphite film - Google Patents
Manufacturing method of high-thermal-conductivity graphite film Download PDFInfo
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- CN104176733A CN104176733A CN201410421775.6A CN201410421775A CN104176733A CN 104176733 A CN104176733 A CN 104176733A CN 201410421775 A CN201410421775 A CN 201410421775A CN 104176733 A CN104176733 A CN 104176733A
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Abstract
The invention discloses a manufacturing method of a high-thermal-conductivity graphite film. The manufacturing method is characterized by comprising the following steps: by taking a polyimide film as a raw material, pre-sintering, and sintering at high temperature to obtain the high-thermal-conductivity graphite film. A graphite flake with the specific gravity of more than 2.0g/cm<3>, thermal diffusivity of 10cm<2>/s and thermal conductivity of more than 1600W/(M*k) is manufactured.
Description
Technical field
The present invention relates to a kind of production technology of the graphite film for heat conduction and heat radiation, particularly a kind of manufacture method of high conductive graphite film.
Background technology
Along with electron device and product are to the development in high integration, high computing field, wasted power doubles thereupon, and heat radiation becomes a urgent need to solve the problem day by day.
At present, various heat sink materials are widely used.Dissimilar heat sink material, can have different performances, such as the heat conductivility of metallic substance is good, particularly a part of metallic substance wherein, and as copper, aluminium, silver etc., its thermal conductivity is especially good.Utilize these metal scatterers, such as the scatterer of copper scatterer, aluminium matter, be widely used.
Due to scientific and technological development, above-mentioned metallic substance, as heat conductor processing, cannot meet, the demand that electron trade is highly integrated, thereby there is the synthetic graphite mould material of high heat dispersion, its thermal conductivity is very high, can reach 1500W/mK, and density gently arrives 1g/cm
3～2g/cm
3left and right and there is the feature of high conductivity.In addition, because can alleviating the thickness of film and thering is flexibility, thereby be expected to as the place narrow always, maybe needing heat transfer device material or the radiator material in the place processing through gap.
The application of current high conductive graphite film is more and more extensive, manufacture method for high conductive graphite film is also more and more, have from the natural graphite method that pressing forms in addition, also there is the manufacture method of describing the high conductive graphite film that is processed into from Graphene, and have the manufacture method etc. of the high conductive graphite film of synthetic.
The current method that adopts polyimide to prepare high conductive graphite film is a lot, the for example manufacture method of the disclosed a kind of high conductive graphite film of China Patent Publication No. CN103011141: it adopts Kapton as starting material, through carbonization and two processes of greying, its technological process is as follows: a. selects Kapton as starting material, between each strata imide membrane, sandwiches graphite paper; B. put into charring furnace in nitrogen or ar gas environment carbonization by being separated with the Kapton of graphite paper after cross layered, 1000 DEG C-1400 DEG C of carbonization temperatures, the time is controlled at 1 hour-6 hours; C. after carbonization, carry out greying, greying is also to carry out in nitrogen or ar gas environment, and temperature is controlled at 2500 DEG C to 3000 DEG C left and right, is controlled in 12 hours.
The graphite radiating adhesive tape of the disclosed a kind of high thermal conductivity coefficient of Chinese patent Granted publication CN103059761, comprises a graphite linings, and this graphite linings upper surface is covered with a metal level, and described graphite linings lower surface is coated with heat-conducting glue adhesion coating; Graphite linings obtains by following technique: will in polyamic acid solution, add ethylene glycol or triethylamine; Be warmed up to 300 DEG C and obtain Kapton; Kapton is risen to 250 DEG C, then rise to 1200 DEG C of carbonized film that obtain pre-burned; Adopt the carbonized film of rolling press calendering pre-burned; Be warming up to again after 2400 DEG C, then rise to 2900 DEG C of main graphite films of firing of acquisition; Then thereby the main graphite film of firing is rolled and obtains described graphite linings.
China Patent Publication No. CN103787323 disclosed a kind of heat conduction graphite flake and manufacturing process thereof, heat conduction is made up of Kapton, the first coat and the second coat with graphite flake, and described the first coat, the second coat lay respectively at the upper and lower surface of Kapton; The first coat, the second coat form by graphite modified dose of sintering, the graphite modified dose of component by following weight part forms: 20～25 parts of benzophenone tetracarboxylic dianhydrides, 14～16 parts of pyromellitic acid anhydrides, 22～26 parts of diaminodiphenylmethane, 25～35 parts of dimethyl formamides, 1.8～2.5 parts of ethylene glycol, 2.5～3 parts of polydimethylsiloxanes.
Disclosed a kind of conductive graphite paster for adhesive tape of China Patent Publication No. CN103796493 and preparation method thereof, conductive graphite paster surface-coated has heat-conducting glue adhesion coating; Conductive graphite paster is made up of Kapton, the first coat and the second coat, and described the first coat, the second coat lay respectively at the upper and lower surface of Kapton; Described the first coat, the second coat form by the component of following weight part: 20～25 parts of benzophenone tetracarboxylic dianhydrides, 12～18 parts of pyromellitic acid anhydrides, 20～28 parts of diaminodiphenylmethane, 20～25 parts of dimethyl formamides, 8～10 parts of N-Methyl pyrrolidone, 1.5～2.5 parts of ethylene glycol, 2～3 parts of polydimethylsiloxanes, 0.8～1.5 part of dibutyl phthalate.
The disclosed a kind of conductive graphite paster for microelectronic device of China Patent Publication No. CN103763892, comprises the first heat-conducting glue adhesion coating, graphite linings and the second heat-conducting glue adhesion coating; Graphite linings obtains by following processing method, and this processing method comprises the following steps: all apply graphite modified dose of one deck on the upper and lower surface of the Kapton through step 1 and obtain Kapton after treatment; Kapton after treatment is warming up to 800 DEG C, after insulation, is being warming up to 1200 DEG C of carbonized film that obtain pre-burned; Adopt rolling press to roll the carbonized film of the pre-burned of described step 4; Be warming up to 2400 DEG C, obtain the main graphite film of firing thereby be warming up to again 2900 DEG C after insulation; Thereby the graphite film that then master of step 5 gained fires rolls and obtains described graphite linings.
The disclosed a kind of conductive graphite sheet of China Patent Publication No. CN103770415 and manufacture method thereof, conductive graphite sheet is made up of Kapton, the first coat and the second coat, and described the first coat, the second coat lay respectively at the upper and lower surface of Kapton; The first coat, the second coat form by graphite modified dose of sintering, the graphite modified dose of component by following weight part forms: 20～25 parts of benzophenone tetracarboxylic dianhydrides, 14～16 parts of pyromellitic acid anhydrides, 22～26 parts of diaminodiphenylmethane, 20～25 parts of dimethyl formamides, 8～10 parts of N-Methyl pyrrolidone, 1.8～2.5 parts of ethylene glycol, 2.5～3 parts of polydimethylsiloxanes.
But the standby high conductive graphite film of existing above-mentioned patent system also has weak point, and for example density is still lighter, and thermal diffusivity is lower.
Summary of the invention
The object of the invention is to provide in order to solve above-mentioned the deficiencies in the prior art that a kind of density is higher, thermal diffusivity is higher, the more manufacture method of the high conductive graphite film of large (0.005mm-0.1mm) of thickness regulation range.
To achieve these goals, the manufacture method of a kind of high conductive graphite film provided by the invention, is characterized in that: adopt Kapton as starting material, fire and two processes of high-temperature firing through preparation, reach required high conductive graphite film, its technological process is as follows:
A. preparation is fired
The Kapton of 10～100 μ m is placed in vacuum oven, is evacuated to 10Pa and is warming up to 1500 DEG C by normal temperature under vacuum environment, be incubated and after 2 hours, be cooled to 200 DEG C and then come out of the stove, being wherein warming up to time of 1500 DEG C by normal temperature is 20 hours; In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.
B. high-temperature firing
Step a is prepared to the Kapton of firing to be placed in High Temperature Furnaces Heating Apparatus, be filled with rare gas element, under rare gas element aerosol surrounds, be warming up to 2950 DEG C by normal temperature, be incubated and after 2 hours, be cooled to 200 DEG C and come out of the stove, after coming out of the stove, roll with milling roller the film that high-temperature firing becomes, make proportion 2.0g/cm
3thermal diffusivity 10cm above,
2the above graphite flake of/s, thermal conductivity 1600W/ (Mk), the condition that wherein rolls is as follows: by graphite flake, between two metal high rigidity chromium plating processed roll shafts, by the oil cylinder working-pressure up to 5Mpa, roll shaft speed is up to 4M/min, allow rapidly graphite flake less thick, thereby improve its density.The I of thickness reaches 0.005mm, and density reaches as high as 2.2g/cm
3.By high-temperature firing, the film after gas delivery is exceeding after 2850 DEG C of high-temperature firings, and remaining carbon atom now absorbs heat total combination occurs, and when promoting crystallization, this crystallization structure becomes stratiform.
In a preferred embodiment of the invention, described rare gas element is argon gas.
The manufacture method of high conductive graphite film provided by the invention, preparation technology is simple, can ensure the high-cooling property of graphite film, strengthens its thermal diffusivity, better, quickly the dissipation of heat of electronic product is gone out.
High conductive graphite film provided by the invention can be widely used in electronic chip, power amplifier, isolator, semiconductor element etc. to be had in the electronic product that heat generating components need to dispel the heat.
Embodiment
Below by embodiment, the invention will be further described.
Embodiment 1:
Adopt Kapton as starting material, fire and two processes of high-temperature firing through preparation, reach required high conductive graphite film, its technological process is as follows:
A. preparation is fired
The Kapton of 50 μ m is placed in vacuum oven, is evacuated to that 10Pa is following is warming up to 1500 DEG C by normal temperature under vacuum environment, be incubated and after 2 hours, be cooled to 200 DEG C and then come out of the stove, being wherein warming up to time of 1500 DEG C by normal temperature is 20 hours; In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.
B. high-temperature firing
Step a is prepared to the Kapton of firing to be placed in High Temperature Furnaces Heating Apparatus, be filled with rare gas element, under surrounding, rare gas element aerosol is warming up to 2950 DEG C by normal temperature, be incubated and after 2 hours, be cooled to 200 DEG C and come out of the stove, after coming out of the stove, roll with milling roller the film that high-temperature firing becomes, the condition that wherein rolls is as follows: by graphite flake between two metal high rigidity chromium plating processed roll shafts, by the oil cylinder working-pressure up to 5Mpa, roll shaft speed is up to 4M/min, allows rapidly graphite flake less thick, thereby improves its density.The I of thickness reaches 0.02mm, and density reaches as high as 2.2g/cm
3.By high-temperature firing, the film after gas delivery is exceeding after 2800 DEG C of high-temperature firings, and remaining carbon atom now absorbs heat total combination occurs, and when promoting crystallization, this crystallization structure becomes stratiform.
Test the high conductive graphite film of this embodiment by thickness piece, recording thickness is 0.021mm, tests the high conductive graphite film of this embodiment by specific weight determine instrument, and recording density is 2.15g/cm
3, detect the high conductive graphite film of this embodiment, thermal diffusivity 10.2cm by the resistance to laser heat conducting instrument of speeding (model LFA467)
2/ s, thermal conductivity 1864W/ (Mk).
Embodiment 2:
Adopt Kapton as starting material, fire and two processes of high-temperature firing through preparation, reach required high conductive graphite film, its technological process is as follows:
A. preparation is fired
The Kapton of 25 μ m is placed in vacuum oven, is evacuated to that 10Pa is following is warming up to 1500 DEG C by normal temperature under vacuum environment, be incubated and after 1 hour, be cooled to 200 DEG C and then come out of the stove, being wherein warming up to time of 1500 DEG C by normal temperature is 18 hours; In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.
B. high-temperature firing
Step a is prepared to the Kapton of firing to be placed in High Temperature Furnaces Heating Apparatus, be filled with rare gas element, under surrounding, rare gas element aerosol is warming up to 2950 DEG C by normal temperature, be incubated and after 1.5 hours, be cooled to 200 DEG C and come out of the stove, after coming out of the stove, roll with milling roller the film that high-temperature firing becomes, the condition that wherein rolls is as follows: by graphite flake between two metal high rigidity chromium plating processed roll shafts, by the oil cylinder working-pressure up to 5Mpa, roll shaft speed is up to 4M/min, allows rapidly graphite flake less thick, thereby improves its density.The I of thickness reaches 0.009mm, and density reaches as high as 2.2g/cm
3.By high-temperature firing, the film after gas delivery is exceeding after 2850 DEG C of high-temperature firings, and remaining carbon atom now absorbs heat total combination occurs, and when promoting crystallization, this crystallization structure becomes stratiform.
Test the high conductive graphite film of this embodiment by thickness piece, recording thickness is 0.009mm, tests the high conductive graphite film of this embodiment by specific weight determine instrument, and recording density is 2.18g/cm
3, detect the high conductive graphite film of this embodiment, thermal diffusivity 11.2cm by the resistance to laser heat conducting instrument of speeding (model LFA467)
2/ s, thermal conductivity 2075W/ (Mk).
Embodiment 3:
Adopt Kapton as starting material, fire and two processes of high-temperature firing through preparation, reach required high conductive graphite film, its technological process is as follows:
A. preparation is fired
The Kapton of 75 μ m is placed in vacuum oven, is evacuated to that 10Pa is following is warming up to 1500 DEG C by normal temperature under vacuum environment, be incubated and after 2.5 hours, be cooled to 200 DEG C and then come out of the stove, being wherein warming up to time of 1500 DEG C by normal temperature is 25 hours; In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.
B. high-temperature firing
Step a is prepared to the Kapton of firing to be placed in High Temperature Furnaces Heating Apparatus, be filled with rare gas element, under surrounding, rare gas element aerosol is warming up to 2950 DEG C by normal temperature, be incubated and after 1.5 hours, be cooled to 200 DEG C and come out of the stove, after coming out of the stove, roll with milling roller the film that high-temperature firing becomes, the condition that wherein rolls is as follows: by graphite flake between two metal high rigidity chromium plating processed roll shafts, by the oil cylinder working-pressure up to 5Mpa, roll shaft speed is up to 4M/min, allows rapidly graphite flake less thick, thereby improves its density.The I of thickness reaches 0.03mm, and density reaches as high as 2.2g/cm
3.By high-temperature firing, the film after gas delivery is exceeding after 2850 DEG C of high-temperature firings, and remaining carbon atom now absorbs heat total combination occurs, and when promoting crystallization, this crystallization structure becomes stratiform.
Test the high conductive graphite film of this embodiment by thickness piece, recording thickness is 0.032mm, tests the high conductive graphite film of this embodiment by specific weight determine instrument, and recording density is 2.10g/cm
3, detect the high conductive graphite film of this embodiment, thermal diffusivity 10.1cm by the resistance to laser heat conducting instrument of speeding (model LFA467)
2/ s, thermal conductivity 1802W/ (Mk).
Claims (1)
1. a manufacture method for high conductive graphite film, is characterized in that: adopt Kapton as starting material, fire and two processes of high-temperature firing through preparation, reach required high conductive graphite film, its technological process is as follows:
A. preparation is fired
The Kapton of 10～100 μ m is placed in vacuum oven, is evacuated to 10Pa and is warming up to 1500 DEG C by normal temperature under vacuum environment, be incubated and after 2 hours, be cooled to 200 DEG C and then come out of the stove, being wherein warming up to time of 1500 DEG C by normal temperature is 20 hours; In preparation sintering procedure, Kapton starts 600 DEG C of left and right to decompose, and forms nitrogen-atoms, Sauerstoffatom, the hydrogen atom gasification of polyimide, from Kapton, separates.
B. high-temperature firing
Step a is prepared to the Kapton of firing to be placed in High Temperature Furnaces Heating Apparatus, be filled with rare gas element, under rare gas element aerosol surrounds, be warming up to 2950 DEG C by normal temperature, be incubated and after 2 hours, be cooled to 200 DEG C and come out of the stove, after coming out of the stove, roll with milling roller the film that high-temperature firing becomes, make proportion 2.0g/cm
3thermal diffusivity 10cm above,
2the above graphite flake of/s, thermal conductivity 1600W/ (Mk), the condition that wherein rolls is as follows: by graphite flake, between two metal high rigidity chromium plating processed roll shafts, by the oil cylinder working-pressure up to 5Mpa, roll shaft speed is up to 4M/min, allow rapidly graphite flake less thick, thereby improve its density.The I of thickness reaches 0.005mm, and density reaches as high as 2.2g/cm
3.By high-temperature firing, the film after gas delivery is exceeding after 2850 DEG C of high-temperature firings, and remaining carbon atom now absorbs heat total combination occurs, and when promoting crystallization, this crystallization structure becomes stratiform.
The manufacture method of high conductive graphite film as claimed in claim 1, is characterized in that: described rare gas element is argon gas.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104909358A (en) * | 2015-05-25 | 2015-09-16 | 镇江博昊科技有限公司 | Preparation method of large-size high-heat conduction graphite membrane |
| CN107001048A (en) * | 2014-12-04 | 2017-08-01 | 株式会社钟化 | High vacuum interlayer thermal bonding graphite flake |
| CN107098334A (en) * | 2017-06-19 | 2017-08-29 | 广东思泉新材料股份有限公司 | A kind of method for preparing graphene powder |
| CN109678145A (en) * | 2017-10-18 | 2019-04-26 | 北京大学深圳研究生院 | A kind of graphite microspheres and preparation method thereof |
| CN111886285A (en) * | 2018-03-22 | 2020-11-03 | 聚酰亚胺先端材料有限公司 | Polyimide film including omni-directional polymer chain, method of manufacturing the same, and graphite sheet manufactured using the same |
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| CN107001048A (en) * | 2014-12-04 | 2017-08-01 | 株式会社钟化 | High vacuum interlayer thermal bonding graphite flake |
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