CN109536142A - A kind of preparation method of graphene film Heat Conduction Material - Google Patents
A kind of preparation method of graphene film Heat Conduction Material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of graphene film Heat Conduction Material, for substituting the artificial graphite cooling fin using PI as raw material.The preparation method of the graphene film Heat Conduction Material includes: 1, graphene-thermal conductive ceramic-polymer compound film preparation；2, graphene-thermal conductive ceramic-polymer compound film is by graphitization fabrication process；3, calendering process.Graphene-thermal conductive ceramic-polymer compound film preparation: by using watersoluble plumbago alkene and minute quantity nonionic surface active agent and aqueous high molecular shape film auxiliary agent, and thermal conductive ceramic nano-powder dispersion liquid, the slurry of viscosity 1000-5000cps is prepared into pure aquatic system, then by slurry curtain coating on release film, it is made after drying tunnel is dry, graphitization fabrication process includes heating, crystallization treatment, three sections of natural cooling processing.This preparation method processing procedure is simple, product thermal coefficient is high while environmentally friendly, and overall process does not generate harmful toxic matter.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene film Heat Conduction Material, belong to heat conduction and heat radiation material technical field.
Background technique
With the high speed development of electronic technology, the concentration of electronic component is also higher and higher, and power device is all
There is certain stabilized operating temperature section, however the highly dense of device means that having a large amount of heat generates.Therefore, how
It is effective to realize device heat dissipation, to guarantee the stable operation of device, also more it is concerned by people.
Traditional heat sink material is mainly metal material, and graphite material is wide due to its high-termal conductivity, low-density
It is general to be applied in dissipation from electronic devices material.Wherein conduction graphite film not only has thermally conductive system more higher than metals such as aluminium, copper
Number, lower density, and it can be smoothly attached to any plane and curved surface, therefore for such as mobile phone, plate electricity
The electronic products such as brain, LED illumination device and wearable device, conduction graphite film are relatively popular heat dissipation pad pastings.Especially
It is that OLED screen curtain is quickly grown in recent years, the big factory of three magnitudes has had large scale OLED screen curtain that will put into volume production, and market is to big
Blowout will occur in the demand of breadth conduction graphite film.
At present there are three ways to commercialization preparation conduction graphite film, first, macromolecule PI film by high temperature pyrolysis and
Oriented graphite film is formed after graphitization；Second, obtaining graphite film after graphite expansion is rolled；Third, a small amount of graphite microchip is added
It is added to macromolecule and obtains graphite film by graphitization processing after middle mixing film forming.The graphite film thermal conductivity that method 1 obtains reaches
1600 W/ (mK), but it can be used for graphited PI film higher cost, the process is more complicated.This method obtains simultaneously
Graphite film breadth is generally in 200mm or hereinafter, the application in terms of large scale OLED screen curtain heat dissipation is limited.Although 2 cost of method
It is lower, but graphite film thermal conductivity only has 500-800 W/ (mK), can not meet electronic product and has increasingly improved to heat dissipation
Demand.Method 3 is improved in method 1, replaces PI with other high molecular materials, then passes through addition graphene filling
Piece, to reach the purpose for improving thermal conductivity.But body material or high molecular material, film in carbonisation still
Fold can be generated due to the ununiform shrinkage after being heated, to cause defect in subsequent graphitizing process, reduce graphitization
Degree, moreover, the graphitization temperature that this method is selected is slightly lower, so that degree of graphitization is also declined, in addition, macromolecule filming
When need that organic solvent is added, be unfavorable for environmental-friendly.Separately have method propose one kind based on inorganic material, organic material be
Auxiliary heat conductivity gap filling material, but its material of main part selected is ceramic powder, thermal coefficient is far away from natural graphite, more not
And the thermal coefficient of graphene, and be difficult to form a film, using limited.Therefore, one kind is developed based on graphene, passes through slurry
Coating obtains big breadth membrane material, and then the method that high temperature prepares graphene film Heat Conduction Material will be such that existing issue is improved.
Summary of the invention
The present invention is intended to provide a kind of preparation method of graphene film Heat Conduction Material, is mainly used for substituting the artificial of PI raw material
Graphite heat radiation fin improves some problems present in existing preparation method.
To realize that aforementioned invention purpose, the technical solution adopted by the present invention are as follows.
Graphene-thermal conductive ceramic-polymer compound film preparation method: watersoluble plumbago alkene is used, with minute quantity nonionic
Type surfactant, aqueous high molecular shape film auxiliary agent and thermal conductive ceramic nano-powder dispersion liquid, through overmulling in pure aquatic system
The slurry that viscosity is 1000-5000 cps is prepared into after conjunction.By slurry curtain coating on release film, graphite is made after drying tunnel is dry
Alkene-thermal conductive ceramic-polymer compound film.The breadth of composite membrane is limited only in the coating width of coating apparatus.
Further, temperature of the graphene-thermal conductive ceramic-polymer compound film when drying tunnel is dry is 50-90
DEG C, the time is 1-6 min.Since the wet-film thickness of coating formation is mostly in 0.1mm or more, lead to wet film in order to avoid temperature is excessively high
Middle moisture boiling, drying tunnel temperature is no more than 90 DEG C, and drying time should not be less than 1min, as far as possible under more mild environment
Remove the moisture in wet film.It is generally acknowledged that floated drying tunnel is optimal selection.
Further, the graphene-thermal conductive ceramic-polymer compound film is with a thickness of 0.02-1.5 mm.At present in intelligence
The most common graphite radiating component thickness is mostly between 0.02-1mm in energy electronic equipment, it is contemplated that high temperature graphitization process and pressure
Graphene film thickness can be declined during prolonging, and control above-mentioned composite film thickness between 0.02-1.5mm most beneficial for subsequent
Processing procedure.
Further, the preparation proportion of the composite membrane are as follows: watersoluble plumbago alkene: nonionic surface active agent: aqueous height
Molecule shape film auxiliary agent: thermal conductive ceramic nano-powder dispersion liquid=(80-95): (1-6): (3-10): (1-4) (mass ratio).
Further, the nonionic surfactant is octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, laurel
Any one in alcohol polyoxyethylene ether；Aqueous high molecular shape film auxiliary agent is polyvinyl alcohol, hydroxypropyl methyl cellulose, methylol
Fiber receives, any one in hydroxyethyl cellulose；Thermal conductive ceramic nano-powder is aluminum oxide, any one in boron nitride
Kind.
Further, in the graphene-thermal conductive ceramic-polymer compound film preparation method, for mixing aqueous stone
Black alkene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent and thermal conductive ceramic nano-powder method include: that machinery stirs
It mixes, one of ultrasonic mixing, ball milling mixing or any two kinds or more of combination.Wherein nonionic surface active agent is used for
Disperse aqueous graphene, so that graphene exists in the slurry with lamellar morphology, and then also with sheet in the composite membrane of preparation
Form exists, and lamellar morphology is easily formed the graphite flake layer of larger size during graphitization processing, so that ultimately forming
Heat Conduction Material have better heating conduction.Aqueous high molecular shape film auxiliary agent facilitates slurry and is formed after coating with certain
The composite membrane of toughness, convenient for removing and rewinding.These surfactants and shape film auxiliary agent can be present in graphitizing process simultaneously
Low-temperature zone cracks to form coke, and high temperature section can be also graphitized, and will not bring flaw to final products.Thermal conductive ceramic nano-powder
Play the role of similar with surfactant, main is also that graphene is promoted to disperse in the slurry with laminated structure.Surface-active
Agent can be played with thermal conductive ceramic nano-powder and cooperate with peptizaiton, and more preferably than one-component, while ceramic powder is in stone for effect
When inkization high temperature section is pyrolyzed, similar catalyst action can be played and promote to reconnect between graphene film and piece.
Further, according to the mixed method, the lateral dimension of the watersoluble plumbago alkene after mixing in slurry is 10-70
μm, longitudinal size is 10-70 μm, with a thickness of 0.4-6 nm.
Further, above-mentioned graphene-thermal conductive ceramic-polymer compound film need to be removed from release film, at rewinding
Reason obtains bottomless film coiled material.
Further, bottomless film coiled material need to could obtain graphene film Heat Conduction Material by graphitization processing.Graphitization system
Journey technique is broadly divided into three sections: heating, crystallization treatment and cooling, specific procedure are as follows: 0-1000 DEG C with 4-8 DEG C/min heating
Rate heating, 1000-1600 DEG C with 3-4 DEG C/min heating rate heating, 1600-2300 DEG C with 1-2 DEG C/min heat up speed
Rate heating, 2300-2900 DEG C with 4-6 DEG C/min heating rate heating, 2900-3100 DEG C by 1-12 h crystallization treatment, from
So it is cooled to room temperature.
Above-mentioned technological parameter is mainly according to a kind of existing technology of our company " preparation work of uniform high thermal conductivity graphite film coiled material
Skill, 201711158854.2 " do partial adjustment.
Further, the coiled material after graphitization is carried out cold-pressed steel roll-in to prolong, obtains the uniform continuity graphene of thickness
Film Heat Conduction Material.
Further, the graphene film Heat Conduction Material with a thickness of 20-100 μm, thermal conductivity is 1000-1800 W/
(m·K)。
Compared with prior art, the present invention has the advantage that as follows.
1, raw material is graphene aqueous liquid dispersion, and China is graphene producing country the biggest in the world at present, and raw material supply is reliable
Stablize, is not in cause to stop production because of starving.And the current whole world graphite PI only has ten Yu Jia suppliers, raw material
It is under one's control.
2, bulk is graphene, is no longer needed to by special carbonization treatment, preparation process is simpler, can directly carry out
Graphitization processing；Final finished thickness, breadth can be customized according to customer demand simultaneously, and especially thickness and breadth is much better than PI
Graphite flake: larger thickness can reduce the fitting number of plies, and then reduce fitting double-sided adhesive and bear to component overall thermal conductivity
Face is rung；Big breadth can then make large-sized radiating subassembly, the heat dissipation suitable for large scale OLED screen curtain.Therefore the present invention produces
Product applicability is better than the graphite flake of PI raw material.
3, properties of product meet or exceed PI raw graphite piece, and horizontal thermal conductivity factor can achieve same with PI raw graphite piece
Etc. levels, and vertical direction thermal coefficient is much better than PI raw graphite piece, is meeting the needs of horizontal thermal diffusion simultaneously, vertical thermal
Diffusivity is stronger.
4, cost is better than PI raw graphite piece: current domestic watersoluble plumbago alkene unit price and graphite PI are essentially identical, and this hair
Bright procedure for producing is simpler, energy consumption is lower, the yield of a procedure also will due to the two procedures yield of PI graphite flake, thus
Overall cost has advantage.Simultaneously as graphene film thickness of the invention can achieve twice or more of traditional PI graphite flake,
It can be reduced in radiating subassembly manufacturing process for cross cutting link and be die cut and be bonded number, rejection rate can be reduced for down-stream enterprise
It reduces cost and improves yield, create more values.
Specific embodiment
Specific description is done to the present invention below in conjunction with specific implementation example.Certainly, following instance is that the present invention is real
A part in example.
Embodiment 1.
Graphene-thermal conductive ceramic-polymer compound film quality composition and ratio is as follows: watersoluble plumbago alkene: non-ionic table
Face activating agent: aqueous high molecular shape film auxiliary agent: thermal conductive ceramic nano-powder=95:1:3:1, wherein the maximum of watersoluble plumbago alkene is straight
Diameter is 50 μm, and maximum gauge is 6 nm, and nonionic surfactant selects octyl phenol polyoxyethylene ether, aqueous high molecular shape film
Agent is hydroxypropyl methyl cellulose, and ceramic powder is aluminum oxide (D50 partial size is 5 μm).
Graphene film Heat Conduction Material preparation step is as follows.
Step 1: graphene-thermal conductive ceramic-polymer compound film preparation, comprising the following steps: first by watersoluble plumbago
Alkene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent, thermal conductive ceramic nano-powder are added in blender, stirring
Time is 20 min, forms the slurry that viscosity is 2000 cps.It then is 80 through excess temperature by slurry curtain coating on release film
DEG C dry 3 min of drying tunnel after graphene-thermal conductive ceramic-polymer compound film with a thickness of 80 μm is made.
Step 2: above-mentioned graphene-thermal conductive ceramic-polymer compound film is removed from release film, is obtained through rewinding processing
Obtain bottomless film coiled material.Then bottomless film coiled material is subjected to graphitization fabrication process, specific procedure are as follows: by coiled material with 6 DEG C/min liter
Warm rate is raised to 1000 DEG C from room temperature, and then 4 DEG C/min heating rate is raised to 1600 DEG C, then with 2 DEG C/min heating rate
2300 DEG C are raised to, then is raised to 2950 DEG C with 5 DEG C/min heating rate, then the natural cooling after 2950 DEG C of 8 h of holding.Most
The coiled material after graphitization is carried out cold-pressed steel roll-in afterwards to prolong, it is thermally conductive to obtain the uniform continuity large scale package graphene film of thickness
Material.
Graphene film Heat Conduction Material obtained by above-mentioned technique with a thickness of 45 μm, thermal conductivity is 1300 W/ (mK).
Embodiment 2.
Graphene-thermal conductive ceramic-polymer compound film quality composition and ratio is as follows: watersoluble plumbago alkene: non-ionic table
Face activating agent: aqueous high molecular shape film auxiliary agent: thermal conductive ceramic nano-powder=90:3:6:1, wherein the maximum of watersoluble plumbago alkene is straight
Diameter is 70 μm, and maximum gauge is 3 nm, and nonionic surfactant selects octyl phenol polyoxyethylene ether, aqueous high molecular shape film
Agent is hydroxypropyl methyl cellulose, and ceramic powder is aluminum oxide (D50 partial size is 15 μm).
Graphene film Heat Conduction Material preparation step is as follows.
Step 1: graphene-thermal conductive ceramic-polymer compound film preparation, comprising the following steps: first by watersoluble plumbago
Alkene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent, thermal conductive ceramic nano-powder are added in blender, stirring
Time is 20 min, forms the slurry that viscosity is 5000 cps.It then is 60 through excess temperature by slurry curtain coating on release film
DEG C dry 6 min of drying tunnel after graphene-thermal conductive ceramic-polymer compound film with a thickness of 1.5 mm is made.
Step 2: above-mentioned graphene-thermal conductive ceramic-polymer compound film is peeled from release film, is obtained through rewinding processing
Obtain bottomless film coiled material.Then bottomless film coiled material is subjected to graphitization fabrication process, specific procedure are as follows: by coiled material with 6 DEG C/min liter
Warm rate is raised to 1000 DEG C from room temperature, and then 4 DEG C/min heating rate is raised to 1600 DEG C, then with 2 DEG C/min heating rate
2300 DEG C are raised to, then is raised to 2950 DEG C with 5 DEG C/min heating rate, then the natural cooling after 2950 DEG C of 8 h of holding.Most
The coiled material after graphitization is carried out cold-pressed steel roll-in afterwards to prolong, it is thermally conductive to obtain the uniform continuity large scale package graphene film of thickness
Material.
Graphene film Heat Conduction Material obtained by above-mentioned technique with a thickness of 1 mm, thermal conductivity is 1000 W/ (mK).
Embodiment 3.
Graphene-thermal conductive ceramic-polymer compound film quality composition and ratio is as follows: watersoluble plumbago alkene: non-ionic table
Face activating agent: aqueous high molecular shape film auxiliary agent: thermal conductive ceramic nano-powder=85:5:9:1, wherein the diameter of watersoluble plumbago alkene divides
Cloth is 10-15 μm, and maximum gauge is 0.4 nm, and nonionic surfactant selects octyl phenol polyoxyethylene ether, aqueous high molecular
Shape film is received for hydroxylmethyl cellulose, and ceramic powder is boron nitride (D50 partial size is 1 um).
Graphene film Heat Conduction Material preparation step is as follows.
Step 1: graphene-thermal conductive ceramic polymer compound film preparation, comprising the following steps: first by watersoluble plumbago
Alkene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent, thermal conductive ceramic nano-powder are added in blender, stirring
Time is 20 min, forms the slurry that viscosity is 1000 cps.It then is 90 through excess temperature by slurry curtain coating on release film
DEG C dry 1 min of drying tunnel after graphene-thermal conductive ceramic-polymer compound film with a thickness of 20 μm is made.
Step 2: above-mentioned graphene-thermal conductive ceramic-polymer compound film is removed from release film, is obtained through rewinding processing
Obtain bottomless film coiled material.Then bottomless film coiled material is subjected to graphitization fabrication process, specific procedure are as follows: by coiled material with 6 DEG C/min liter
Warm rate is raised to 1000 DEG C from room temperature, and then 4 DEG C/min heating rate is raised to 1600 DEG C, then with 2 DEG C/min heating rate
2300 DEG C are raised to, then is raised to 2950 DEG C with 5 DEG C/min heating rate, then the natural cooling after 2950 DEG C of 8 h of holding.Most
The coiled material after graphitization is carried out cold-pressed steel roll-in afterwards to prolong, it is thermally conductive to obtain the uniform continuity large scale package graphene film of thickness
Material.
Graphene film Heat Conduction Material obtained by above-mentioned technique with a thickness of 0.02 mm, thermal conductivity is 1800 W/ (mK).
Embodiment 4.
Graphene-thermal conductive ceramic-polymer compound film quality composition and ratio is as follows: watersoluble plumbago alkene: non-ionic table
Face activating agent: aqueous high molecular shape film auxiliary agent: thermal conductive ceramic nano-powder=80:6:10:4, wherein the diameter of watersoluble plumbago alkene divides
Cloth is 20-45 μm, and maximum gauge is 5 nm, and nonionic surfactant selects octyl phenol polyoxyethylene ether, aqueous high molecular shape
Film is received for hydroxylmethyl cellulose, and ceramic powder is boron nitride (D50 partial size is 5 μm).
Graphene film Heat Conduction Material preparation step is as follows.
Step 1: graphene-thermal conductive ceramic polymer compound film preparation, comprising the following steps: first by watersoluble plumbago
Alkene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent, thermal conductive ceramic nano-powder are added in blender, stirring
Time is 20 min, forms the slurry that viscosity is 5000 cps.It then is 80 through excess temperature by slurry curtain coating on release film
DEG C dry 3 min of drying tunnel after graphene-thermal conductive ceramic-polymer compound film with a thickness of 0.25 mm is made.
Step 2: above-mentioned graphene-thermal conductive ceramic-polymer compound film is removed from release film, is obtained through rewinding processing
Obtain bottomless film coiled material.Then bottomless film coiled material is subjected to graphitization fabrication process, specific procedure are as follows: will carbonization coiled material with 6 DEG C/
Min heating rate is raised to 1000 DEG C from room temperature, and then 4 DEG C/min heating rate is raised to 1600 DEG C, then with 2 DEG C/min heating
Rate is raised to 2300 DEG C, then is raised to 2950 DEG C with 5 DEG C/min heating rate, then naturally cold after 2950 DEG C of 8 h of holding
But.The coiled material after graphitization is finally carried out cold-pressed steel roll-in to prolong, obtains the uniform continuity large scale package graphene of thickness
Film Heat Conduction Material.
Graphene film Heat Conduction Material obtained by above-mentioned technique with a thickness of 0.11 mm, thermal conductivity is 1100 W/ (mK).
Technical solution of the present invention is elaborated through having gone for the above specific implementation case, it should be understood that above to implement
Example is concrete case of the invention, includes but is not limited only to this, all to meet spirit of that invention, make within the scope of the present invention
Modification and improvement, should belong to the scope of the present invention.
Claims (11)
1. a kind of preparation method of graphene film Heat Conduction Material, it is characterised in that include following preparation step:
Step 1: graphene-thermal conductive ceramic-polymer compound film preparation；
Raw material composition and quality proportioning are as follows: watersoluble plumbago alkene: nonionic surface active agent: aqueous high molecular shape film auxiliary agent: lead
Thermal Ceramics nano-powder dispersion liquid=(80-95): (1-6): (3-10): (1-4)；
Above-mentioned raw materials are prepared into after mixing to the slurry of viscosity 1000-5000 cps in pure aquatic system, slurry is cast
On release film, graphene-thermal conductive ceramic-polymer compound film is made after drying tunnel is dry；Later by the thermally conductive pottery of graphene-
Porcelain-polymer compound film is removed from release film, then obtains bottomless film coiled material through rewinding processing；
Step 2: graphitization fabrication process；
Above-mentioned bottomless film coiled material is carried out graphitization fabrication process by following procedure: 0-1000 DEG C with 4-8 DEG C/min heating speed
Rate heating, 1000-1600 DEG C with the heating of 3-4 DEG C/min heating rate, 1600-2300 DEG C with 1-2 DEG C/min heating rate
Heating, 2300-2900 DEG C with 4-6 DEG C/min heating rate heating, 2900-3100 DEG C pass through 1-12 h crystallization treatment, nature
It is cooled to room temperature；
Step 3: calendering process；
Coiled material progress cold-pressed steel roll-in after graphitization fabrication process is prolonged and is led to get to the uniform continuity graphene film of thickness
Hot material.
2. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, it is characterised in that: described aqueous
The graphene film number of plies of graphene is no more than 15 layers, and the diameter of single graphene diaphragm is between 10-70 μm.
3. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, it is characterised in that: it is described it is non-from
Subtype surfactant and aqueous high molecular shape film auxiliary agent can be in 800 DEG C or less pyrolysis completely.
4. a kind of preparation method of graphene film Heat Conduction Material according to claims 1 or 3, it is characterised in that: described
Nonionic surfactant is octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, any in ethoxylated dodecyl alcohol
It is a kind of.
5. a kind of preparation method of graphene film Heat Conduction Material according to claims 1 or 3, it is characterised in that: described
Aqueous high molecular shape film auxiliary agent is polyvinyl alcohol, in hydroxypropyl methyl cellulose, sodium cellulose glycolate, hydroxyethyl cellulose
Any one.
6. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, it is characterised in that: described thermally conductive
Ceramic nano-powder body is aluminum oxide, any one in boron nitride.
7. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, which is characterized in that the drying tunnel
Drying temperature is 50-90 DEG C, and the time is 1-6 min.
8. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, which is characterized in that the graphite
Alkene-thermal conductive ceramic-polymer compound film is with a thickness of 0.02-1.5 mm.
9. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, it is characterised in that: for aqueous
Graphene, nonionic surface active agent, aqueous high molecular shape film auxiliary agent and thermal conductive ceramic nano-powder mixed method include
The combination of one of mechanical stirring, ultrasonic mixing, ball milling mixing or any two kinds or more.
10. a kind of preparation method of graphene film Heat Conduction Material according to claim 1, which is characterized in that after mixing
The lateral dimension of watersoluble plumbago alkene in slurry is 10-70 μm, and longitudinal size is 10-70 μm, with a thickness of 0.4-6 nm.
11. according to the preparation method of graphene film Heat Conduction Material described in claims 1, it is characterised in that the graphene
Film Heat Conduction Material with a thickness of 20-100 μm, thermal conductivity is 1000-1800 W/ (mK).
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