CN103011141A - Method for manufacturing high thermal conductivity graphite film - Google Patents
Method for manufacturing high thermal conductivity graphite film Download PDFInfo
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- CN103011141A CN103011141A CN2012105576348A CN201210557634A CN103011141A CN 103011141 A CN103011141 A CN 103011141A CN 2012105576348 A CN2012105576348 A CN 2012105576348A CN 201210557634 A CN201210557634 A CN 201210557634A CN 103011141 A CN103011141 A CN 103011141A
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- kapton
- carbonization
- graphite film
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 77
- 239000010439 graphite Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000003763 carbonization Methods 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001721 polyimide Polymers 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 150000002505 iron Chemical class 0.000 claims description 18
- 239000012266 salt solution Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 10
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000007858 starting material Substances 0.000 claims description 9
- 150000003949 imides Chemical class 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 4
- 238000005452 bending Methods 0.000 abstract description 6
- 238000005087 graphitization Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract 2
- 230000017525 heat dissipation Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for manufacturing a high thermal conductivity graphite film, which adopts polyimide films as raw materials and is formed through two processes of carbonization and graphitization. The technological processes of the high thermal conductivity graphite film comprise the steps as follows: a, the polyimide films are selected as the raw materials, and a piece of graphite paper is clamped between each layer of the polyimide films; b, the polyimide films which are provided with the graphite paper at intervals, crossed and stacked are placed into a carbonization furnace to be carbonized in an environment of nitrogen or argon, the carbonized temperature ranges from 1000 DEG C to 1400 DEG C, and the time is controlled from 1 hour to 6 hours; and c, after the carbonization, the graphitization is performed also in the environment of nitrogen or argon, the temperature is controlled in a range from about 2500 DEG C to 3000 DEG C, and the time is controlled within 12 hours. The method for manufacturing the high thermal conductivity graphite film has a simple manufacturing process, the high heat dissipation capacity of the graphite film is guaranteed, the bending-resistant performance is enhanced, and a requirement for a thin and light electronic product of a consumer is met to a certain extent.
Description
Technical field
The present invention relates to a kind of production technology of the graphite film for heat conduction and heat radiation, particularly the manufacture method of high conductive graphite film.
Background technology
Along with the development to high integration, high computing field of electron device and product, 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, a part of metallic substance wherein particularly, and as copper, aluminium, silver etc., its thermal conductivity is especially good.Utilize these metal scatterers, the scatterer such as copper scatterer, aluminium matter, be widely used.Its correlation parameter is as follows
| Material | Thermal conductivity W/mK | Specific heat capacity J/kgK | Density g/cm3 |
| Aluminium | 200 | 880 | 2.7 |
| Copper | 380 | 385 | 8.96 |
Due to scientific and technological development, above-mentioned metallic substance is processed as heat conductor, can't meet, the demand that electron trade is highly integrated, thereby the synthetic graphite mould material of high heat dispersion appearred, its thermal conductivity is very high, can reach 1500W/mK, and density is gently to 1 g/cm3～2g/cm3 left and right and have characteristics of high conductivity.In addition, because of the thickness that can alleviate film and there is flexibility, thereby be expected to always as in narrow place, maybe need heat transfer device material or the radiator material in the place that processes 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, the manufacture method of describing the high conductive graphite film be processed into from Graphene is also arranged, and the manufacture method etc. that the high conductive graphite film of synthetic is arranged.
But existing high conductive graphite film also has weak point, though high conductive graphite film has certain folding resistance, the weak strength between material, can be torn easily, or because of the displacement of institute's adhesive attachment means, disrepair phenomenon occurs, or entry material comes off etc.
The high-cooling property that how effectively to keep graphite film strengthens its resistance to bend(ing) energy simultaneously, can resist larger External Force Acting, and being needs the problem solved at present.
Summary of the invention
The objective of the invention is provides a kind of preparation technology simple in order to solve above-mentioned the deficiencies in the prior art, both kept graphite film high-cooling property, strengthen its resistance to bend(ing) energy, can resist again the manufacture method of the high conductive graphite film of larger External Force Acting.
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, through carbonization and two processes of greying, reach required high conductive graphite film, its technological process is as follows:
A. select Kapton as starting material, Kapton and graphite paper cut into specified dimension, put into definite height by the polyimide film layer that cuts into specified dimension is stacked, sandwich graphite paper between each strata imide membrane, make Kapton and graphite paper form cross-level stacked; At this, the high heat conduction of graphite paper can make film be heated evenly in carbonization process, and stack height can be determined according to the height of carbide furnace;
B. will between be separated with the Kapton of graphite paper after cross layered and put into charring furnace and carry out carbonization, be filled with nitrogen or argon gas during carbonization in carbide furnace, make Kapton carbonization in nitrogen or ar gas environment, wherein carbonization time is raised to 1000 ℃-1400 ℃ from room temperature, and the time is controlled at 1 hour-6 hours in; Under the environment of inert body, to constantly be filled with nitrogen or argon gas to discharge oxygen or hydrogen etc. in carbonization process;
C. carry out greying after carbonization, greying is also to carry out in nitrogen or ar gas environment, in this environment, the carbon molecule is rearranged into to graphite-structure, and temperature is controlled at 2500 ℃ to 3000 ℃ left and right, is controlled in 12 hours.
Described Kapton thickness is at 25 microns-125 microns; Described graphite paper thickness is at 0.2 millimeter-3 millimeters.
Graphited temperature is controlled at 2600 ℃-2800 ℃, and the time is controlled at 1 hour-6 hours, and the greying environment adopts ar gas environment.But the low nitrogen of available rates, do not had hydrogen, oxygen composition in its environment in graphitizing process yet, and after greying, film can stand repeatedly bending and not break.
First spray iron salt solutions on Kapton before to the Kapton carbonization, then carry out the crossing stack with graphite paper.Described iron salt solutions can be: iron(ic) chloride, iron nitrate and iron sulphide are made into mixed molysite, and the ratio of weight part is: 30 parts-40 parts, iron(ic) chloride, 40 parts-50 parts of iron nitrates, 10 parts-20 parts, iron sulphide; Mixed molysite is dissolved in methanol solution, and the wherein wt ratio is respectively: 5 parts to 10 parts of mixed molysites, 95 parts to 90 parts of methanol solutions; Be made into thus iron salt solutions.All gasify and overflow due at high temperature chlorine, nitrogen, oxygen, sulphur after the Kapton greying of spraying iron salt solutions, stay iron also between the graphite after greying, more easily make thus the high conductive graphite rete layer obtained separate.
The manufacture method of high conductive graphite film provided by the invention, preparation technology is simple, can guarantee the high-cooling property of graphite film, strengthen its resistance to bend(ing) energy, allow electronic equipment can realize miniaturization, slimming and lightness, and can be widely used in less gap and nonisulated environment, met to a certain extent human consumer's demand not only thin but also light to electronic product, also can save more transportation cost for the client simultaneously.Graphite film provided by the invention can be widely used in heat conduction film and the radiator material of electronics, precision equipment etc., is a kind of have good resistance to bend(ing), graphite film that thermal diffusivity is good.And size dimension can be accomplished 350mm*350mm, even larger.
Conductive graphite film properties index provided by the invention is as follows:
1) thickness degree scope is from 0.0125mm to 0.075mm
2) the thermal conductivity plane is to >=1450 ± 200W/mK: vertically to 5 ± 0.5W/mK
3) density g/cm
3: 1.8-2.0
Embodiment
Below by embodiment, the invention will be further described.
Embodiment 1:
The manufacture method of the high conductive graphite film of the present embodiment, adopt Kapton as starting material, through carbonization and two processes of greying, reaches required high conductive graphite film, and its technological process is as follows:
A, selection Kapton are as starting material, Kapton and graphite paper cut into specified dimension, put into definite height by the polyimide film layer that cuts into specified dimension is stacked, sandwich graphite paper between each strata imide membrane, make Kapton and graphite paper form cross-level stacked; Stack height is determined according to the height of carbide furnace;
B, will between be separated with the Kapton of graphite paper after cross layered and put into charring furnace and carry out carbonization, be filled with nitrogen during carbonization in carbide furnace, make Kapton carbonization in nitrogen environment, wherein carbonization is raised to 1000 ℃ from room temperature, and 1000 ℃ of lower carbonization times are controlled 6 hours;
Carry out greying after c, carbonization, greying is carried out in ar gas environment, and temperature is controlled at 2500 ℃, and graphitization time is controlled at 6 hours.
Described Kapton thickness is 25 microns; Graphite paper thickness is at 0.2 millimeter.
The high conductive graphite film obtained thus, the about 0.0125mm of thickness; The thermal conductivity plane is to>=1450W/mK; Vertically to 5 W/mK; Density g/cm3:1.8
.through 10,000 bendings, do not break.
Embodiment 2:
The manufacture method of the high conductive graphite film that the present embodiment is described, adopt Kapton as starting material, between each strata imide membrane, sandwiches graphite paper, and wherein Kapton thickness is 125 microns; Graphite paper thickness is at 3 millimeters.Be filled with argon gas during carbonization in carbide furnace, make Kapton carbonization in ar gas environment, 1400 ℃ of carbonization temperatures, 1400 ℃ of lower carbonization times are controlled 1 hour; Greying is carried out in nitrogen environment, and temperature is controlled at 3000 ℃, and graphitization time is controlled at 3 hours.The high conductive graphite film obtained thus, the about 0.075mm of thickness; The thermal conductivity plane is to>=1650W/mK: vertically to 5.5 W/mK density g/cm3:2.0
.through 10,000 bendings, do not break.
Embodiment 3:
The manufacture method of the high conductive graphite film that the present embodiment is described, adopt Kapton as starting material, between each strata imide membrane, sandwiches graphite paper, and wherein Kapton thickness is 50 microns; Graphite paper thickness is at 1 millimeter.Be filled with nitrogen during carbonization in carbide furnace, make Kapton carbonization in nitrogen environment, 1200 ℃ of carbonization temperatures, 1200 ℃ of lower carbonization times are controlled 3 hours; Greying is carried out in ar gas environment, and temperature is controlled at 2800 ℃, and graphitization time is controlled at 5 hours.The high conductive graphite film obtained thus, the about 0.03mm of thickness; The thermal conductivity plane is to>=1600W/mK: vertically to 5.3 W/mK density g/cm3:1.95
.through 10,000 bendings, do not break.
Embodiment 4:
The manufacture method of the high conductive graphite film that the present embodiment is described, adopt Kapton as starting material, between each strata imide membrane, sandwiches graphite paper, and wherein Kapton thickness is: 80 microns; Graphite paper thickness is at 1 millimeter.Be filled with nitrogen during carbonization in carbide furnace, make Kapton carbonization in nitrogen environment, 1300 ℃ of carbonization temperatures, 1300 ℃ of lower carbonization times are controlled 4 hours; Greying is carried out in ar gas environment, and temperature is controlled at 2700 ℃, and graphitization time is controlled at 4 hours.
The present embodiment is first to spray iron salt solutions on Kapton before to the Kapton carbonization, then carries out the crossing stack with graphite paper.Described iron salt solutions is: iron(ic) chloride, iron nitrate and iron sulphide are made into mixed molysite, and the ratio of weight part is: 30 parts, iron(ic) chloride, 40 parts of iron nitrates, 20 parts, iron sulphide; Mixed molysite is dissolved in methanol solution, and the wherein wt ratio is respectively: 5 parts of mixed molysites, 95 parts of methanol solutions; Be made into thus iron salt solutions.All gasify and overflow due at high temperature chlorine, nitrogen, oxygen, sulphur after the Kapton greying of spraying iron salt solutions, stay iron also between the graphite after greying, make the high conductive graphite film obtained be easy to separate layer by layer.
The high conductive graphite film obtained thus, the about 0.035mm of thickness; The thermal conductivity plane is to>=1600W/mK: vertically to 5.3 W/mK; Density g/cm3:1.95
.through 5000 bendings, do not break.
Embodiment 5:
The present embodiment is to provide for spraying iron salt solutions on Kapton, and described iron salt solutions is: iron(ic) chloride, iron nitrate and iron sulphide are made into mixed molysite, and the ratio of weight part is: 40 parts, iron(ic) chloride, 50 parts of iron nitrates, 10 parts, iron sulphide; Mixed molysite is dissolved in methanol solution, and the wherein wt ratio is respectively: 10 parts of mixed molysites, 90 parts of methanol solutions; Be made into thus iron salt solutions.After the Kapton greying of spraying iron salt solutions, stay the iron amount between graphite linings to increase, the high conductive graphite film obtained more easily separates layer by layer.But mixed molysite different ratios and just contribute to reduce costs and can contribute to the high conductive graphite film obtained easily to be separated into layer by layer target with the proportioning of methyl alcohol, be proven can play in scope provided by the invention and contribute to the segregative target of graphite film, again can minimum cost, do not remake in the present embodiment detailed proportioning for example for this reason.
Claims (7)
1. the manufacture method of a high conductive graphite film is characterized in that: adopt Kapton as starting material, through carbonization and two processes of greying, reach required high conductive graphite film, its technological process is as follows:
Select Kapton as starting material, Kapton and graphite paper cut into specified dimension, put into definite height by the polyimide film layer that cuts into specified dimension is stacked, sandwich graphite paper between each strata imide membrane, make Kapton and graphite paper form cross-level stacked;
Put into charring furnace and carry out carbonization being separated with the Kapton of graphite paper after cross layered, be filled with nitrogen or argon gas during carbonization in carbide furnace, make Kapton carbonization in nitrogen or ar gas environment, wherein carbonization time is raised to 1000 ℃-1400 ℃ from room temperature, and the time is controlled at 1 hour-6 hours in;
Carry out greying after carbonization, greying is also to carry out in nitrogen or ar gas environment, and temperature is controlled at 2500 ℃ to 3000 ℃ left and right, is controlled in 12 hours.
2. the manufacture method of high conductive graphite film according to claim 1, it is characterized in that: described Kapton thickness is at 25 microns-125 microns; Described graphite paper thickness is at 0.2 millimeter-3 millimeters.
3. the manufacture method of high conductive graphite film according to claim 1 and 2, it is characterized in that: graphited temperature is controlled at 2600 ℃-2800 ℃, and the time is controlled at 1 hour-6 hours, and the greying environment adopts ar gas environment.
4. the manufacture method of high conductive graphite film according to claim 1 and 2 is characterized in that: first spray iron salt solutions on Kapton before to the Kapton carbonization, then carry out the crossing stack with graphite paper.
5. the manufacture method of high conductive graphite film according to claim 3 is characterized in that: first spray iron salt solutions on Kapton before to the Kapton carbonization, then carry out the crossing stack with graphite paper.
6. the manufacture method of high conductive graphite film according to claim 4, it is characterized in that described iron salt solutions is: iron(ic) chloride, iron nitrate and iron sulphide are made into mixed molysite, the ratio of weight part is: 30 parts-40 parts, iron(ic) chloride, 40 parts-50 parts of iron nitrates, 10 parts-20 parts, iron sulphide; Mixed molysite is dissolved in methanol solution, and the wherein wt ratio is respectively: 5 parts to 10 parts of mixed molysites, 95 parts to 90 parts of methanol solutions; Be made into thus iron salt solutions.
7. the manufacture method of high conductive graphite film according to claim 5, it is characterized in that described iron salt solutions is: iron(ic) chloride, iron nitrate and iron sulphide are made into mixed molysite, the ratio of weight part is: 30 parts-40 parts, iron(ic) chloride, 40 parts-50 parts of iron nitrates, 10 parts-20 parts, iron sulphide; Mixed molysite is dissolved in methanol solution, and the wherein wt ratio is respectively: 5 parts to 10 parts of mixed molysites, 95 parts to 90 parts of methanol solutions; Be made into thus iron salt solutions.
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| CN2012105576348A CN103011141A (en) | 2012-12-20 | 2012-12-20 | Method for manufacturing high thermal conductivity graphite film |
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| CN2012105576348A CN103011141A (en) | 2012-12-20 | 2012-12-20 | Method for manufacturing high thermal conductivity graphite film |
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