CN107686109A - A kind of preparation method of the double-deck carbon-based heat conduction film of high performance graphite graphene - Google Patents
A kind of preparation method of the double-deck carbon-based heat conduction film of high performance graphite graphene Download PDFInfo
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- CN107686109A CN107686109A CN201710582407.3A CN201710582407A CN107686109A CN 107686109 A CN107686109 A CN 107686109A CN 201710582407 A CN201710582407 A CN 201710582407A CN 107686109 A CN107686109 A CN 107686109A
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Abstract
The present invention relates to a kind of preparation method of the carbon-based heat conduction film of bilayer, step are as follows：(1) preparation of graphene-based slurry：A. the solution that graphene oxide (GO) will be included carries out hydrothermal reduction reaction, and graphene-based slurry is prepared in ball milling afterwards；Or graphene-based slurry is prepared with the method for mechanical stripping in the solution comprising graphite by b.；(2) preparation of heat conduction film：By the graphene-based slurry of preparation coated on graphite paper, heat conduction film is obtained.The film constructed not only maintains the good mechanical performance of graphite paper.Compared to single graphite paper, the heat-sinking capability for being coated with the double-deck carbon-based heat conduction film of graphene improves 30%, realizes 400W m‑1k‑1The capacity of heat transmission above.Using coating methods such as spread coating, spraying process, knife coating, print processes by the graphene-based slurry of preparation coated on commercial graphite paper, technique is simple, is advantageous to mass produce.
Description
Technical field
The invention belongs to technical field of nano material, more particularly, to a kind of preparation side of the carbon-based heat conduction film of bilayer
Method.
Background technology
With the fast development of science and technology, high-efficiency heat conduction and radiating turn into many field urgent problems to be solved.Such as
The high power electronic equipment of communications satellite can produce and gather in the process of running substantial amounts of heat.Highly integrated electronics device
Part (such as CPU), the caloric value of its unit volume electronic device can increase rapidly with the increase of working time, therefore can make system
Caused heat abruptly increase.If processing is not in time, it may result in semiconductor devices premature aging or accelerate the heat of electronic component
Mechanical failure.Therefore in order to meet electronic equipment high power, the product design main trend of small size, there is an urgent need to develop a germplasm
The material that amount is light, thermal conductivity is high.
Gold and silver belong to the optimal material of heat conductivility in traditional metal thermal conductive material, but its price is too high, it is difficult to quilt
Extensive use.Metallic copper also has a preferable radiating effect, but it has and is oxidized easily and reduces the limitations such as performance.In addition,
In space industry, small device has high thermal conductivity and high-temperature capability necessary not only for Heat Conduction Material, also to have good
Thermomechanical property and less density.
Current many scientists, which recognize to produce using the special construction and performance of carbon material, meets above-mentioned requirements
Highly heat-conductive material.Carbon material has relatively low density, low thermal coefficient of expansion, excellent mechanical performance and higher thermal conductivity,
It is a kind of Heat Conduction Material most with prospects in recent years, thus in the energy, computing technique, communication, electronics, laser and space section
Etc. field has broad application prospects.But the normal temperature thermal conductivity of general polycrystalline graphite material is only 70~150W m-1K-1, far can not meet the needs of above-mentioned occasion.
Therefore, constructing a kind of carbon-based High-performance heat conduction material of new structure urgently needs.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of system of the carbon-based heat conduction film of bilayer
Preparation Method, there are at least 400W m according to the heat conduction film prepared by this method-1k-1Thermal conductivity, wherein by reaction raw materials
Selected and the critical process step such as the preparation to graphene slurry and the selection of painting method improvement, realize novel double-layer
The preparation of carbon-based heat conduction film；Also, the preparation method technique is simple, simple operation, reaction material is cheap, is easy to get, Er Qieke
To prepare on a large scale.
Technical solution of the present invention is as follows：
A kind of preparation method of the carbon-based heat conduction film of bilayer, comprises the following steps：
(1) preparation of graphene-based slurry：
A. the solution that graphene oxide (GO) will be included carries out hydrothermal reduction reaction, and ball milling is prepared graphene-based afterwards
Slurry；Or
B. graphene-based slurry is prepared with the method for mechanical stripping in the solution comprising graphite；
(2) preparation of heat conduction film：The graphene-based slurry that step (1) is prepared obtains coated on graphite paper
Heat conduction film.
According to the present invention, in step (1) a, carbon nanometer can also be included in the solution comprising graphene oxide (GO)
One or more in the materials such as pipe, diamond, carborundum, silicon, gold, silver, copper, aluminium.
According to the present invention, in step (1) b, surface dispersant, for example, 12 are also included in the solution comprising graphite
Sodium alkyl benzene sulfonate, sodium stearyl sulfate, hexadecyltrimethylammonium chloride, polyvinyl alcohol, polyvinylpyrrolidone, carboxylic first
At least one of base sodium cellulosate and polyethylene glycol.
According to the present invention, in step (1) b, after being peeled off with the method for mechanical stripping, can optionally with CNT, Buddha's warrior attendant
One or more mixing in the materials such as stone, carborundum, silicon, gold, silver, copper, aluminium, are prepared graphene composite mortar；
According to the present invention, in step (1) a, the time of the ball milling is 1~10h, preferably 2~5h, more preferably 3h.
According to the present invention, in step (1) a, the concentration of the graphene oxide is 0.01mg/ml-50mg/ml.
According to the present invention, in step (1) a, the reaction temperature is 160 DEG C~200 DEG C, preferably 180 DEG C.
According to the present invention, in step (1) a, the reaction time is 4~10h, preferably 5~8h, more preferably 6h.
According to the present invention, in step (2), the painting method includes spread coating, spraying process, knife coating, print process etc..
According to the present invention, in step (2), by the graphene-based slurry of preparation coated in after on graphite paper, including plus
The step of heat, the heating-up temperature are 50 DEG C~110 DEG C, preferably 60 DEG C~100 DEG C.
The present invention also provides a kind of double-deck carbon-based heat conduction film being prepared by the above method.
The present invention also provides a kind of double-deck carbon-based heat conduction film, including graphite paper, and in graphene layer thereon.It is described
Graphene layer optionally also includes the one or more in the materials such as CNT, diamond, carborundum, silicon, gold, silver, copper, aluminium.
Technical scheme compared with prior art, has advantages below：
1. the double-deck carbon-based heat conduction film of the present invention, with reference to graphite paper and highly conductive, heat conduction graphene, makes it have more
Good heat transfer and heat-sinking capability.The film not only maintains the good mechanical performance of graphite paper.Moreover, with single graphite paper
Compare, the heat-sinking capability for being coated with the double-deck carbon-based heat conduction film of graphene improves 30%, realizes 400W m-1k-1More than
The capacity of heat transmission.
2. the present invention uses graphene oxide or graphite as raw material, graphene is prepared by the methods of reduction or mechanical stripping
Based sizing.
3. the present invention is using spread coating, spraying process, the coating method such as knife coating, print process by the graphene-based slurry of preparation
Coated on commercial graphite paper, technique is simple, is advantageous to mass produce.
Brief description of the drawings
Fig. 1 is the double-deck carbon-based heat conduction membrane structure schematic diagram of graphite-graphene.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.Furthermore, it is to be understood that after content disclosed in this invention has been read, ability
Field technique personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the protection that the present invention is limited
Within the scope of.
Embodiment 1
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL), it is put into 100mL autoclave, at 180 DEG C
React 6h；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water, be finally putting into ball milling in ball mill
3h。
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with knife coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 402W m-1k-1。
Embodiment 2
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL) and 70mg CNT ultrasonic mixings, it is put into 100mL's
In autoclave, 6h is reacted at 180 DEG C；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL
Water, it is finally putting into ball milling 3h in ball mill.
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with knife coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 493W m-1k-1。
Embodiment 3
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL) and 70mg silicon-carbide particle ultrasonic mixings, it is put into 100mL
Autoclave in, react 6h at 180 DEG C；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL
Water, it is finally putting into ball milling 3h in ball mill.
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with knife coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 420W m-1k-1。
Embodiment 4
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL) and 70mg silicon grain ultrasonic mixings, it is put into 100mL height
Press in reactor, react 6h at 180 DEG C；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water,
It is finally putting into ball milling 3h in ball mill.
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with knife coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 412W m-1k-1。
Embodiment 5
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL) and 70mg Argent grain ultrasonic mixings, it is put into 100mL height
Press in reactor, react 6h at 180 DEG C；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water,
It is finally putting into ball milling 3h in ball mill.
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with knife coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 446W m-1k-1。
Embodiment 6
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL), it is put into 100mL autoclave, at 180 DEG C
React 6h；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water, be finally putting into ball milling in ball mill
3h。
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with spread coating, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 409W m-1k-1。
Embodiment 7
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL), it is put into 100mL autoclave, at 180 DEG C
React 6h；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water, be finally putting into ball milling in ball mill
3h。
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with print process, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 406W m-1k-1。
Embodiment 8
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL), it is put into 100mL autoclave, at 180 DEG C
React 6h；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL water, be finally putting into ball milling in ball mill
3h。
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with spraying process, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 413W m-1k-1。
Embodiment 9
The preparation of double-deck carbon-based heat conduction film：
(1) by 70mL graphene oxide water solution (2mg/mL) and 70mg silicon-carbide particle ultrasonic mixings, it is put into 100mL
Autoclave in, react 6h at 180 DEG C；After cooling, deposit is centrifuged, supernatant is removed and then adds 10mL
Water, it is finally putting into ball milling 3h in ball mill.
(2) the graphene-based slurry being prepared in step (1) is coated uniformly on graphite paper with print process, at 60 DEG C
Drying, that is, obtain double-layer carbon base heat conduction film, the heat conduction thermal conductivity of thin film is 417W m-1k-1。
Embodiment 10
The preparation of double-deck carbon-based heat conduction film：
(1) a certain amount of graphite, a certain amount of surface dispersant and a certain amount of water are by mechanically pulling off preparation quality
Content is 1-15% graphene-based slurry.
(2) graphene-based slurry is coated uniformly on graphite paper with print process, is dried at 100 DEG C, that is, obtain double-layer carbon
Base heat conduction film, the heat conduction thermal conductivity of thin film are 412W m-1k-1。
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above-mentioned embodiment.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., it should be included in the guarantor of the present invention
Within the scope of shield.
Claims (10)
1. a kind of preparation method of the carbon-based heat conduction film of bilayer, it is characterised in that comprise the following steps：
(1) preparation of graphene-based slurry：
A. the solution that graphene oxide (GO) will be included carries out hydrothermal reduction reaction, and graphene-based slurry is prepared in ball milling afterwards
Material；Or
B. graphene-based slurry is prepared with the method for mechanical stripping in the solution comprising graphite；
(2) preparation of heat conduction film：The graphene-based slurry that step (1) is prepared obtains heat conduction coated on graphite paper
Film.
2. according to the method for claim 1, it is characterised in that described comprising graphene oxide (GO) in step (1) a
The one or more in the materials such as CNT, diamond, carborundum, silicon, gold, silver, copper, aluminium can also be included in solution.
3. method according to claim 1 or 2, it is characterised in that in step (1) b, in the solution comprising graphite also
Including surface dispersant, for example, neopelex, sodium stearyl sulfate, hexadecyltrimethylammonium chloride, poly-
At least one of vinyl alcohol, polyvinylpyrrolidone, sodium carboxymethylcellulose and polyethylene glycol.
4. according to the method any one of claim 1-3, it is characterised in that in step (1) a, the time of the ball milling
For 1~10h, preferably 2~5h, more preferably 3h.
5. according to the method any one of claim 1-4, it is characterised in that in step (1) a, the graphene oxide
Concentration be 0.01mg/ml-50mg/ml.
6. according to the method any one of claim 1-5, it is characterised in that in step (1) a, the reaction temperature is
160 DEG C~200 DEG C, preferably 180 DEG C.
7. according to the method any one of claim 1-6, it is characterised in that in step (1) a, the reaction time is 4
~10h, preferably 5~8h, more preferably 6h.
8. according to the method any one of claim 1-7, it is characterised in that in step (2), the painting method includes
Spread coating, spraying process, knife coating, print process；
Preferably, after the graphene-based slurry of preparation is coated on graphite paper, in addition to the step of heating, the heating temperature
Spend for 50 DEG C~110 DEG C, preferably 60 DEG C~100 DEG C.
9. the double-deck carbon-based heat conduction film being prepared as the method any one of claim 1-8.
10. a kind of double-deck carbon-based heat conduction film, including graphite paper, and it is optional in graphene layer thereon, the graphene layer
Also include the one or more in the materials such as CNT, diamond, carborundum, silicon, gold, silver, copper, aluminium.
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| CN109968846A (en) * | 2019-04-30 | 2019-07-05 | 山东华滋自动化技术股份有限公司 | A kind of graphene coating process |
| CN111233515A (en) * | 2020-03-19 | 2020-06-05 | 北京晶龙特碳科技有限公司 | Method for preparing nano-graphite coating on surface of graphite product |
| CN111944497A (en) * | 2019-05-16 | 2020-11-17 | 常州第六元素材料科技股份有限公司 | Graphene oxide composite carbon source mixture and preparation method thereof, graphene heat-conducting film and preparation method thereof |
| CN115141036A (en) * | 2021-03-29 | 2022-10-04 | 翔名科技股份有限公司 | Graphite assembly and method of making the same |
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