CN106191781A - A kind of preparation method of high heat conduction height heat radiation flexible graphite material - Google Patents
A kind of preparation method of high heat conduction height heat radiation flexible graphite material Download PDFInfo
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- CN106191781A CN106191781A CN201510359807.9A CN201510359807A CN106191781A CN 106191781 A CN106191781 A CN 106191781A CN 201510359807 A CN201510359807 A CN 201510359807A CN 106191781 A CN106191781 A CN 106191781A
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- flexible graphite
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- graphite material
- heat radiation
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- 230000005855 radiation Effects 0.000 title claims abstract description 23
- 239000007770 graphite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 30
- 239000010439 graphite Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000010408 film Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000013528 metallic particle Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 229920002799 BoPET Polymers 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000004544 sputter deposition Methods 0.000 claims abstract description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 description 13
- 239000002131 composite material Substances 0.000 description 11
- 239000004020 conductor Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000002657 fibrous material Substances 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920013657 polymer matrix composite Polymers 0.000 description 2
- 239000011160 polymer matrix composite Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The preparation method of a kind of high heat conduction height heat radiation flexible graphite material, relates to the preparation method of a kind of graphite material, mainly comprises the steps of step one: made the superficial growth layer of metal thin film of flexible graphite platelet by methods such as sputtering, chemistry；Step 2: heat in a vacuum so that metallic film becomes metallic particles；Step 3: be passed through hydrogen, in a vacuum continuous heating；Step 4: close hydrogen, be passed through organic gas post-heating；Step 5: resulting materials is combined with PET film.The present invention strengthens the effect of heat radiation outside surface red while keeping graphite flake high heat-conducting effect, can i.e. can reach preferable radiating effect without metal heat sink, be greatly reduced the volume of electronic device, and the extensively application to soft graphite has great importance.
Description
Technical field
The present invention relates to the preparation method of a kind of graphite material, particularly relate to the preparation method of a kind of high heat conduction height heat radiation flexible graphite material.
Background technology
Development along with modern science and technology, instrument, equipment, the design of parts, production are towards miniaturization, lightweight, densification, efficient development, the high power density feature of the electronic device that the development of super large-scale integration is again simultaneously is more and more obvious, thus can produce substantial amounts of heat, and these heats can directly influence job stability and the security reliability of electronic device.Therefore, along with increasingly extensive civilian, industrial emissions demand, heat radiation, heat conduction have become the big problem of industrial technology development.Highly heat-conductive material is proposed urgent demand.Highly heat-conductive material brings new technical scheme to this field by a series of different thermal managements.Such as it is widely used in the various great-power electronic chip coolings such as flat faced display, mobile phone, LED substrate and passes through highly heat-conductive material, more excellent heat conductivility is provided in the case of alleviating device weight.At present, strict difinition be there is no for highly heat-conductive material, owing to the metal material such as copper, aluminum is to use relatively broad heat sink or radiator material, these metal materials are as the good conductor of heat, thermal conductivity is in the scope of 200 ~ 400W/mk, in consideration of it, it is generally acknowledged that thermal conductivity can be described as highly heat-conductive material at the material of 200 ~ 400W/mk scope.
At present, highly heat-conductive material mainly has metal-base composites, based composite material of carbon, polymer matrix composites, ceramic matric composite.The thermal conductance of metal material is good, but thermal coefficient of expansion is higher limits its application as heat sink material, it is added thereto to the low filler grain of thermal coefficient of expansion and metal-base composites made by fiber, not only make the thermal coefficient of expansion reduction of metal but also make hot property obtain a certain degree of improvement.It mainly includes Carbon fibe reinforced aluminum matrix composites, Cu-base composites.But the thermal conductivity of metal-base composites depends on the condition of the kind of filler, content, heat treatment, also affected by fiber/matrix interfacial structure simultaneously.Thermal conductivity is relatively low to be also not sufficiently stable.Being applied to of polymer matrix composites and ceramic matric composite is studied less, and material prepared by existing technology, and thermal conductance is the most limited.Applying most is based composite material of carbon.Such as carbon graphite material, highly directional pyrolytic material, high conductive graphite thin film, carbon/carbon composite etc..The flexible graphite material of high heat conduction height heat radiation is that a kind of brand-new in based composite material of carbon leads (dissipating) hot material, has crystal grain orientation and the surface nanofibre shape material with carbon element structure of uniqueness.The production technology of soft graphite is mainly native graphite calendering and synthetic at present.Wherein, native graphite calendering low cost, heat-conducting effect is poor, and synthetic conductive graphite good heat conduction effect, but cost is high, is tens times of native graphite, but the most merely lateral good heat conduction effect of synthetic conductive graphite, longitudinal heat conduction is very poor, dispels the heat hardly.
Summary of the invention
In order to overcome problem above, the present invention strengthens the effect of heat radiation outside surface red while keeping graphite flake high heat-conducting effect, can i.e. can reach preferable radiating effect without metal heat sink, be greatly reduced the volume of electronic device, the extensively application to soft graphite has great importance.
In order to reach object above, on the basis of the soft graphite of molding, the present invention uses the method for PCVD (PCVD) to solve the problems referred to above, the concrete technical scheme of the present invention is: the preparation method of a kind of high heat conduction height heat radiation flexible graphite material, comprises the steps of step one: made the superficial growth layer of metal thin film of flexible graphite platelet by the method such as ion sputtering, chemistry；Step 2: heat in a vacuum so that metallic film becomes metallic particles；Step 3: be passed through hydrogen, in a vacuum continuous heating；Step 4: close hydrogen, be passed through organic gas post-heating；Step 5: resulting materials is combined with PET film.
Optimally, described flexible graphite platelet be horizontal heat conductivity be the natural or artificial flexible graphite platelet of 300 more than W/mK.
Optimally, described metallic film is the thin film such as copper, nickel, ferrum, cobalt.
Optimally, the thickness of described metallic film is 5 ~ 50 nanometers.
Optimally, the vacuum of step 2 is less than 10pa, and heating-up temperature is 300 ~ 900 DEG C, and heat time heating time is 5 ~ 20 minutes.
Optimally, the vacuum in step 3 is 50 ~ 400pa, and heating-up temperature is 300 ~ 900 DEG C, and heat time heating time is 30 ~ 120 minutes.
Optimally, described organic gas is methane, acetylene, propane etc..
Optimally, in step 4, heating-up temperature is 500 ~ 900 DEG C, and heat time heating time is 5 ~ 30 minutes.
In step 2, metallic film can become metallic particles；In step 3, metallic particles is the equal of catalyst, and soft graphite can decompose under the catalytic action of metal, and metal nanoparticle can embed soft graphite surface；In step 4, after heating, uniform nanometer fibrous material with carbon element can be gone out in soft graphite superficial growth, and these nanometer fibrous material with carbon elements can make carbon fiber, CNT etc..In step 5, after compound to prepared material and PET film, i.e. can get the flexible graphite material of high heat conduction height heat radiation.During use, surface has the side of nanofiber material with carbon element to be radiating segment, and opposite side is then thermal source one end.
In the present invention, by the method using PCVD, layer of metal thin film is first sputtered on soft graphite surface, by being thermally formed nano-particle, it is passed through methane again, the gases such as acetylene, form one layer of uniform nanometer fibrous material with carbon element at a certain temperature, good infrared radiating effect can be played, laterally heat conduction can reach 300 ~ more than 1500W/mK, simultaneously, it is that nanofiber material with carbon element dozen increases the specific surface area of graphite and itself just has good infrared radiating effect in heat radiation, so that material surface can i.e. can reach preferable radiating effect without metal heat sink.The present invention had both saved the cost of metal heat sink, reduced again the volume of device, can be widely applied to the heat radiation of electronics and other industry.
Detailed description of the invention
Embodiment one:
Made the Copper thin film of one layer of 5 nanometer of superficial growth of flexible graphite platelet by the method for sputtering, in the vacuum of 5pa vacuum, be heated 5 minutes by the temperature of 300 DEG C, make metallic film become the metallic particles of 5nm.It is passed through hydrogen, under the vacuum pressure of 50pa, continuous heating closes hydrogen after 30 minutes, it is passed through methane to heat 5 minutes at a temperature of 500 DEG C, soft graphite superficial growth can be made to go out uniform nanometer fibrous material, then by resulting materials and PET Film laminated, i.e. can get the high heat conduction height heat radiation flexible graphite material of molding.
Embodiment two:
Made the iron thin film of one layer of 25 nanometer of superficial growth of flexible graphite platelet by the method for sputtering, in the vacuum of 7pa vacuum, be heated 13 minutes by the temperature of 600 DEG C, make metallic film become the metallic particles of 75nm.It is passed through hydrogen, under the vacuum pressure of 250pa, continuous heating closes hydrogen after 80 minutes, it is passed through methane to heat 20 minutes at a temperature of 700 DEG C, soft graphite superficial growth can be made to go out uniform nanometer fibrous material, then by resulting materials and PET Film laminated, i.e. can get the high heat conduction height heat radiation flexible graphite material of molding.
Embodiment three:
Made the Copper thin film of one layer of 50 nanometer of superficial growth of flexible graphite platelet by the method for sputtering, in the vacuum of 9pa vacuum, be heated 20 minutes by the temperature of 900 DEG C, make metallic film become the metallic particles of 150nm.It is passed through hydrogen, under the vacuum pressure of 400pa, continuous heating closes hydrogen after 120 minutes, it is passed through methane to heat 30 minutes at a temperature of 900 DEG C, soft graphite superficial growth can be made to go out uniform nanometer fibrous material, then by resulting materials and PET Film laminated, i.e. can get the high heat conduction height heat radiation flexible graphite material of molding.
The above, be only to presently preferred embodiments of the present invention, be not the restriction that the present invention does other forms, and any those skilled in the art are changed possibly also with the technology contents of the disclosure above or are modified as the Equivalent embodiments of equivalent variations.But, every without departing from the present invention program content, the technical spirit of the foundation present invention, to any simple modification made for any of the above embodiments, equivalent variations and remodeling, still falls within protection scope of the present invention.
Claims (8)
1. the preparation method of one kind high heat conduction height heat radiation flexible graphite material, it is characterised in that comprise the steps of step one: made the superficial growth layer of metal thin film of flexible graphite platelet by the method such as ion sputtering, chemistry；Step 2: heat in a vacuum so that metallic film becomes metallic particles；Step 3: be passed through hydrogen, in a vacuum continuous heating；Step 4: close hydrogen, be passed through organic gas post-heating；Step 5: resulting materials is combined with PET film.
High heat conduction height the most according to claim 1 heat radiation flexible graphite material preparation method, it is characterised in that described flexible graphite platelet be horizontal heat conductivity be the natural or artificial flexible graphite platelet of 300 more than W/mK.
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that described metallic film is the thin film such as copper, nickel, ferrum, cobalt.
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that the thickness of described metallic film is 5 ~ 50 nanometers.
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that the vacuum of step 2 is less than 10pa, and heating-up temperature is 300 ~ 900 DEG C, and heat time heating time is 5 ~ 20 minutes.
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that the vacuum in step 3 is 50 ~ 400pa, and heating-up temperature is 300 ~ 900 DEG C, and heat time heating time is 30 ~ 120 minutes.
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that described organic gas is methane, acetylene, propane etc..
The preparation method of high heat conduction height the most according to claim 1 heat radiation flexible graphite material, it is characterised in that in step 4, heating-up temperature is 500 ~ 900 DEG C, and heat time heating time is 5 ~ 30 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510118330 | 2015-03-18 | ||
| CN2015101183305 | 2015-03-18 |
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| CN106191781A true CN106191781A (en) | 2016-12-07 |
| CN106191781B CN106191781B (en) | 2018-08-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948399A (en) * | 2018-09-29 | 2018-12-07 | 江苏墨泰新材料有限公司 | polymer-graphite composite membrane and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004269319A (en) * | 2003-03-10 | 2004-09-30 | Matsushita Electric Ind Co Ltd | Manufacturing method of foamed graphite sheet |
| US20080171194A1 (en) * | 2007-01-17 | 2008-07-17 | Feng Chia University | Heat dissipation structures |
| CN101865627A (en) * | 2009-04-20 | 2010-10-20 | 华宏新技股份有限公司 | Manufacture method of heat radiation interface device and product thereof |
| CN102791111A (en) * | 2011-05-16 | 2012-11-21 | 华宏新技股份有限公司 | Use of a graphite heat-dissipation device including a plating metal layer |
| CN104029461A (en) * | 2014-06-13 | 2014-09-10 | 江苏悦达新材料科技有限公司 | Graphene/carbon nano tube/graphite film composite material and preparation method thereof |
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- 2015-06-26 CN CN201510359807.9A patent/CN106191781B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004269319A (en) * | 2003-03-10 | 2004-09-30 | Matsushita Electric Ind Co Ltd | Manufacturing method of foamed graphite sheet |
| US20080171194A1 (en) * | 2007-01-17 | 2008-07-17 | Feng Chia University | Heat dissipation structures |
| CN101865627A (en) * | 2009-04-20 | 2010-10-20 | 华宏新技股份有限公司 | Manufacture method of heat radiation interface device and product thereof |
| CN102791111A (en) * | 2011-05-16 | 2012-11-21 | 华宏新技股份有限公司 | Use of a graphite heat-dissipation device including a plating metal layer |
| CN104029461A (en) * | 2014-06-13 | 2014-09-10 | 江苏悦达新材料科技有限公司 | Graphene/carbon nano tube/graphite film composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948399A (en) * | 2018-09-29 | 2018-12-07 | 江苏墨泰新材料有限公司 | polymer-graphite composite membrane and its preparation method and application |
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