CN105111484B - A kind of method of high-efficiency and continuous large area preparation conduction graphite film - Google Patents
A kind of method of high-efficiency and continuous large area preparation conduction graphite film Download PDFInfo
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Abstract
The present invention relates to a kind of methods of high-efficiency and continuous large area preparation heat conductive graphite film, belong to thermally conductive, heat dissipation or soaking technical field of material.The present invention uses continuous rolling graphitization alkene or expanded graphite dispersion liquid or slurry on multilayered structure substrate film, will cover cated substrate film by hot drying tunnel or hot-flow flue, and remove solvent；Then using coating to be compacted to obtained high thermal conductivity graphene or expanded graphite film repeatedly to roll calendar or hydraulic press, in film surface gum or protective film, release paper etc..Obtained graphite film has excellent heating conduction through the invention (horizontal direction thermal coefficient is up to 300~1500W/mK), and can large area batch production, the product in electronic product radiating field, floor heating or the soaking of wall heating system it is thermally conductive on have extraordinary application effect.
Description
Technical field
The present invention relates to a kind of concrete application of graphene or expanded graphite in preparation conduction graphite film, belong to it is thermally conductive,
Heat dissipation or soaking technical field of material.
Background technique
The miniaturization of electronic product now, mobile phone, tablet computer, reader, computer etc., so that the collection of integrated circuit
At Du Genggao, encapsulation requires also higher.But the following heat dissipation problem constrains consumer electronics to thin, light, small, just
Take the developing direction of formula.Before high temperature superconducting materia popularization and application, exploration thermal conductivity is higher, density is small, resistant to high temperature novel
Heat conduction and heat radiation material seems most important.Reliability and service life of the consumer electronics that this material can guarantee etc..
Currently, the graphite or graphite alkenes heat dissipation film main preparation methods sold on the market are macromolecule membrane thermal decomposition method
With thermal expansion graphite rolling process.1. macromolecule membrane thermal decomposition method is mainly to utilize the lesser polyamide of heat-shrinkable (PA), gather
The macromolecules such as sub- amide (PI), polybenzimidazoles (PBI), polypyridobisimidazole (PBBI), polyparaphenylene Asia ethylene (PPV) are thin
Film directly carries out the techniques such as high temperature sintering carbonization-graphitization-calendering and forms.Such as: application No. is 201410421775.6 publication numbers
For CN104176733A a kind of manufacturing method of high thermal conductivity graphite film of Chinese patent using polyimide film as raw material, pass through
Preparation is fired and high temperature fires two processes, and to reach required high thermal conductivity, graphite film density obtained is up to 2.0g/
cm3, thermal coefficient is up to 1600W/mK.Separately there is Chinese patent Authorization Notice No. are as follows: CN103059761A (application number:
CN201210584542.9), CN103787323A (application number: CN201410036030.8), CN103796493A (application number:
CN201410036121.1), CN103763892A (application number: CN201410037378.9), CN103770415A (application number:
It) etc. CN201410038241.5 is all to carry out high temperature sintering carbonization-graphitization-calendering process by raw material of Kapton
Graphite film is made, thermal coefficient highest is also up to 1750W/mK after calendering.Although there is outstanding advantages on heating conduction,
The drawbacks of being these methods is also apparent: high temperature high energy consumption does not meet environmentally protective requirement；Production equipment is required different
It is often harsh, also to lead to inert gas shielding in graphitizing process, yields is not high, is unable to the production of continuity large area so that raw
Produce inefficiency；Raw material sources are few, and at high cost is also one of drawback.2. thermally expanding graphite rolling process mainly with common day
Right graphite composite powder rolls slabbing again after various processing, and general step has hot extruding-removal of impurities-hybrid adhesive-to be rolled into
Piece, such as: application No. is CN201110002281.0, a kind of ultra-thin graphite of the Chinese patent application of Publication No. CN102175089A
Paper cooling fin and its manufacturing method carry out thermal expansion processing, finally through over-voltage using graphite as raw material in 950 DEG C of expansion furnace
Prolong, obtains ultra-thin graphene paper.The most thin thickness of graphene paper is 40 microns, thermal coefficient 300W/mK.Separately have Chinese special
Application No. is CN201210242732.2 (Publication No. CN102730675A), CN201210474790.8 (Publication No. for benefit
CN103387225A), CN201410075835.3 (Publication No. CN103805144A) etc. is carried out preparing in this way and be led
Heat heat dissipation graphite film.Although this method is in high temperature energy consumption and the cost of raw material than having one in macromolecule membrane thermal decomposition method
Fixed advantage, but there is also preparation step complexity is various, can not continuous large-area production, obtained graphite film is in mechanics
The disadvantages of relatively slightly worse in performance and heating conduction.Above-mentioned calendering is common calender calendering, and above-mentioned patent does not also mention
To specifically how rolling and technological parameter.
Summary of the invention
Technical problem solved by the invention is the provision of a kind of preparation conduction graphite film of high-efficiency and continuous large area
Method makes graphene or expanded graphite microplate directional orientation using the roller speed difference of up-down rollers using the technique of orientation roll-in,
Graphite film surface applies cross shear, makes graphene or expanded graphite microplate directional orientation, to obtain the height on horizontal plane
Heating conduction.Its object is to overcome above-mentioned macromolecule membrane thermal decomposition method and thermally expand some disadvantages of graphite rolling process, than
Such as: high energy consumption, process conditions are harsh, yields is low.Production energy consumption is greatly reduced simultaneously under the premise of guaranteeing heating conduction
And cost, the stability and quality of product are improved, it is also possible that the product thickness control of graphite film is being lower than 20 μm of range
It is interior, the conduction graphite film product of excellent cost performance can finally be made.
The present invention provides a kind of preparation conduction graphite film of high-efficiency and continuous large area, which is four layers of knot
Structure, five-layer structure or six layer structure；Wherein, four-layer structure is successively from top to bottom release film or release paper-graphene or expansion
Equadag coating-acrylic compounds adhesive layer-release film；Five-layer structure from top to bottom successively release film or release paper-graphene or swollen
Swollen ultra-thin PET, PI or PEEK high temperature resistant of equadag coating-enhances film-acrylic compounds adhesive layer-release film；Six layer structure by upper and
Under successively release film or release paper-graphene or expanded graphite coating-ultra-thin PET, PI or PEEK high temperature resistant enhance film-acrylic acid
Class adhesive layer-graphene or expanded graphite coating-release film or release paper.
The present invention also provides the method for the preparation conduction graphite film of above-mentioned high-efficiency and continuous large area, technical solution includes
Following steps:
A, graphene or expanded graphite powder the allotment of graphene or expanded graphite dispersion liquid slurry: are distributed to environment-friendly type
In the solution of (containing water-soluble or ethyl alcohol are molten) adhesive, adhesive is controlled with the mass ratio of graphene or expanded graphite powder to protect
Suitable viscosity is demonstrate,proved suitable for roller coating technology.
B, multilayered structure substrate film selects: substrate film is three layers or five-layer structure, material is poly terephthalic acid
Glycol ester (PET) or polyimide (PI) or polyether-ether-ketone (PEEK) macromolecule membrane and acrylic compounds adhesive.
C, roller coating, drying and orientation rolling process: roller coating technology is enterprising using the viscous layer of multilayered structure substrate film
The operation of the deployed graphene of Line Continuity roller coating or expanded graphite dispersion liquid slurry.Wherein, drying process is that have roller coating
The substrate film of graphene or expanded graphite coating carries out drying and processing, then carries out one or many orientation roll-ins to film,
Keep graphene or expanded graphite coating more compact closely knit, crystal grain orientation is regular；Ultra-thin adhesive layer or table are enclosed in coating surface again
Surface protective film.
The graphene is single-layer or multi-layer laminated structure；
The expanded graphite is the worm laminated structure graphite that expansion multiple is greater than 100 times；
The Environment-friendlyadhesive adhesive is that water-soluble or ethyl alcohol colloidal sol sticks agent solution, and the preferred waterglass of Environment-friendlyadhesive adhesive is molten
Liquid, butadiene-styrene rubber/carboxymethyl cellulose lotion, nature rubber latex, acrylonitrile-butadiene rubber latex, butadiene rubber lotion, polytetrafluoroethyl-ne
Aqueous solution, polyvinyl alcohol water solution, acrylic acid/esters class lotion, polyaminoester emulsion or hydroxyethyl cellulose ethyl alcohol are molten
Liquid.
The mass ratio of the graphene or expanded graphite powder and adhesive is 4:1~10:1；
In a preferred embodiment of the invention, the mass ratio of Graphene powder weight and ptfe emulsion solute
4:1。
In another preferred embodiment of the invention, the mass ratio of Graphene powder weight and nature rubber latex solute
9:1。
In another preferred embodiment of the invention, the mass ratio of Graphene powder weight and polyvinyl alcohol aqueous solute
9.5:1。
In another preferred embodiment of the invention, the quality of expanded graphite powder quality and acrylonitrile-butadiene rubber latex solute
Compare 8.5:1.
In another preferred embodiment of the invention, the quality of Graphene powder weight and butadiene rubber lotion liquid solute
Compare 10:1.
The suitable roller coating technology viscosity is 3000mPas~10000mPas.
The substrate film three-decker are as follows: upper layer is the PET release film of 0.15~0.03mm, centre for 0.006~
The propylene acids adhesive layer of 0.03mm, lower layer are PET release layer of the thickness in 0.01~0.05mm；
The substrate film five-layer structure is successively are as follows: upper layer is the PET release film of 0.15~0.03mm, and intermediate three layers are
Two sides is coated with resistance to 200 DEG C of PI or PEEK of 0.01~0.05mm of the propylene acids adhesive of 0.001~0.005mm thickness
The film of high temperature, the bottom are the PET release film layer of 0.01~0.05mm.
The PET release film is a kind of commonly used material of thermal transfer, and ground is PET, forms institute by coating silicone oil
To be also silicon oil membrane.General thickness is from 25um to 150um.Be divided into it is cold and hot tear with the mute face of light, by antistatic and anti-scratch injury
Reason, product have good adsorptivity and stickiness.
The propylene acids adhesive layer, refers to and is coated with propylene acids adhesive layer.
PI film, Kapton (PolyimideFilm) they are the film class insulating materials that performance is best in the world, by
Pyromellitic acid anhydride (PMDA) and diaminodiphenyl ether (DDE) are in intensive polar solvent through polycondensation and casting film-forming is again through imines
Change.
PEEK film, PEEK refer to polyether-ether-ketone, English name poly-ether ether ketone (abbreviation PEEK),
It is the Linear aromatic macromolecular compound in molecular backbone containing chain link.Its component unit is oxygen-to phenylene-oxygen-carbonyl-
It is hemicrystalline, thermoplastic to phenylene.PEEK film refers to the film being pressed by PEEK.
The roller coating technology, which mainly passes through, adjusts pressure pump and roller speed, by graphene or expanded graphite dispersion liquid
Or slurry is coated uniformly on substrate film；The drying process is removal solvent, dry using heated-air drying or hot drying tunnel
Dry, temperature is 90~120 DEG C；The orientation roll-in is that the substrate coated with graphene or expanded graphite coating after drying is thin
Film passes through 2~5 roll-ins under upper and lower each pair of roller differential roller speed ratio, and upper and lower each pair of roller roller Transmission Ratio Control is in 1.5:1~1:
1, pressure is controlled in 20~50MPa, and thickness can be controlled in 10~80 μm, is attached to it on viscous layer of substrate film；It is described
Graphene or expanded graphite coating surface protective film generally use the release film or release paper of environment-friendly type.
The conduction graphite film final finished form are as follows: four-layer structure or five-layer structure or six layer structure.Wherein, four layers
Structure is successively from top to bottom release film or release paper-graphene or expanded graphite coating-acrylic compounds adhesive layer-release film；
Five-layer structure from top to bottom successively release film or release paper-graphene or expanded graphite coating-resistance to height of ultra-thin PET, PI or PEEK
Temperature enhancing film-acrylic compounds adhesive layer-release film.Six layer structure from top to bottom successively release film or release paper-graphene or swollen
Swollen ultra-thin PET, PI or PEEK high temperature resistant of equadag coating-enhances film-acrylic compounds adhesive layer-graphene or expanded graphite coating-
Release film or release paper.
Beneficial effect
Preparation process of the present invention is simple, large area easy to process and large-scale production, carries out to film one or many
Orientation orientation roll-in, keeps graphene or expanded graphite coating more compact closely knit, and crystal grain orientation is regular, overcomes macromolecule membrane heat
It the shortcomings that high temperature highly energy-consuming of decomposition method and thermal expansion graphite rolling process, Gao Chengben, low yields, is made using the method for the present invention
Thermally conductive laminated film can improve very well and improve the performance of common graphite piece, make it have ultra-thin thickness, high-termal conductivity etc.
Advantage.
Detailed description of the invention
Fig. 1 present invention process flow diagram
Specific embodiment
The present invention is described in detail with reference to embodiments, but the present embodiment cannot be used for the limitation present invention, all
Using similar method and its similar variation of the invention, protection scope of the present invention should all be included in.
Embodiment 1
As shown in Figure 1, the number of plies for weighing 1kg first is the graphene powder (N008-P) of 5~8 layers of graphene, by its point
It is dissipated in ptfe emulsion, the mass ratio 4:1 of Graphene powder weight and ptfe emulsion solute is controlled, through defibrination
Machine defibrination, centre can add water to adjust the viscosity of slurry, and control viscosity is 6000mPas.The slurry of milled is poured into roller coating system again
In the low level storage tank of system, pressure revolution speed 50r/min is adjusted, electronic roller coating idler wheel revolving speed 40r/min is adjusted, makes electronic roller coating
Wheel surface sufficiently infiltrates in high-order reservoir, is stained with slurry, then will tear single-sided parting film off, exposes the substrate of viscous layer
(commercially available) the abutting roller coating wheel of loaded film carries out roller coating operation.There is the film of slurry to pass through hot wind drying tunnel or hot drying tunnel, temperature load
Control be 110 DEG C, drying removing dispersing agent, by remove dispersing agent and load there is the film of slurry solids to pass through one or multi-channel pressure
Prolong roller and carry out orientation roll-in, controlling each pair of roller roller speed ratio up and down is 1:1, and pressure is controlled in 20MPa, is finally pasted in coating surface
Close PET protection film (commercially available).Experimental products, with a thickness of 80 μm, are marked according to ASTM D374 standard testing according to ASTM E1461
The thermal coefficient that standard is surveyed is up to 300W/mK.
Wherein roll coating system be by low level fluid reservoir, infusion pump, perfusion tube, special construction high-order reservoir, electromotive roller
Apply this few part composition of wheel.
Embodiment 2
The number of plies for weighing 1kg first is the graphene powder (N006-P) of 3~5 layers of graphene, is dispersed to natural rubber
In latex solution, the mass ratio 9:1 of Graphene powder weight and nature rubber latex solute is controlled, through paste mill grinding, centre can
Water is added to adjust the viscosity of slurry, control viscosity is 4000mPas.The slurry of milled is poured into roll coating system low level storage tank again
In, pressure revolution speed 60r/min is adjusted, electronic roller coating idler wheel revolving speed 60r/min is adjusted, stores up electronic roller coating wheel surface in a high position
It is sufficiently infiltrated in liquid bath, is stained with slurry, then will tear single-sided parting film off, the base load film (commercially available) for exposing viscous layer is tight
It pastes roller coating wheel and carries out roller coating operation.There is the film of slurry by hot wind drying tunnel or hot drying tunnel load, temperature control is 100 DEG C, is dried
Dry removing dispersing agent, by remove dispersing agent and loading has the film of slurry solids to carry out orientation roller by one or multi-channel stack
Pressure, controlling each pair of roller roller speed ratio up and down is 1.1:1, and pressure is controlled in 50MPa, is finally bonded upper PET protection in coating surface
Film (commercially available).Experimental products according to ASTM D374 standard testing with a thickness of 65 μm, according to the thermally conductive system of ASTM E1461 standard testing
Number is up to 600W/mK.
Embodiment 3
The graphene powder (N002-PDR) for weighing 1kg single-layer graphene first, is dispersed to polyvinyl alcohol water solution
In, the mass ratio 9.5:1 of Graphene powder weight and polyvinyl alcohol aqueous solute is controlled, through paste mill grinding, centre can add water
The viscosity of slurry is adjusted, control viscosity is 3000mPas.The slurry of milled is poured into roll coating system low level storage tank again, is adjusted
Pressure revolution speed 40r/min is saved, electronic roller coating idler wheel revolving speed 80r/min is adjusted, makes electronic roller coating wheel surface in high-order reservoir
In sufficiently infiltrate, be stained with slurry, then will tear single-sided parting film off, expose (commercially available) the abutting roller of base load film of viscous layer
It applies wheel and carries out roller coating operation.There is the film of slurry by hot wind drying tunnel or hot drying tunnel load, temperature control is 115 DEG C, and drying is de-
Except dispersing agent, by remove dispersing agent and loading has the film of slurry solids to carry out orientation roll-in by one or multi-channel stack,
The roller speed ratio for controlling each pair of roller up and down is 1.5:1, and pressure is controlled in 40MPa, is finally bonded upper PET protection film in coating surface
(commercially available).Experimental products according to ASTM D374 standard testing with a thickness of 10 μm, according to ASTM E1461 standard testing thermal coefficient
Up to 1500W/mK.
Embodiment 4
The powder (300 mesh expanded graphite powder of Qingdao Xing Yuan aquadag Co., Ltd) for weighing 1kg expanded graphite first, by it
It is dispersed in acrylonitrile-butadiene rubber latex, the mass ratio 8.5:1 of expanded graphite powder quality and acrylonitrile-butadiene rubber latex solute is controlled, through grinding
Pulp grinder defibrination, centre can add water to adjust the viscosity of slurry, and control viscosity is 3500mPas.The slurry of milled is poured into roller coating again
In system low level storage tank, pressure revolution speed 55r/min is adjusted, electronic roller coating idler wheel revolving speed 70r/min is adjusted, makes electronic roller coating
Wheel surface sufficiently infiltrates in high-order reservoir, is stained with slurry, then will tear single-sided parting film off, exposes the substrate of viscous layer
(commercially available) the abutting roller coating wheel of loaded film carries out roller coating operation.There is the film of slurry to pass through hot wind drying tunnel or hot drying tunnel, temperature load
Control be 95 DEG C, drying removing dispersing agent, by remove dispersing agent and load there is the film of slurry solids to pass through one or multi-channel pressure
Prolong roller and carry out orientation roll-in, the roller speed ratio for controlling each pair of roller up and down is 1.2:1, and pressure is controlled in 40MPa, finally in coating table
Face paste closes PET protection film (commercially available).Experimental products according to ASTM D374 standard testing with a thickness of 50 μm, according to ASTM E1461
Standard testing thermal coefficient is up to 500W/mK.
Embodiment 5
The number of plies for weighing 1kg first is the graphene powder (N006-P) of 3~5 layers of graphene, is dispersed to along fourth rubber
In latex solution, the mass ratio 10:1 of Graphene powder weight and butadiene rubber lotion solute is controlled, through paste mill grinding, centre can
Water is added to adjust the viscosity of slurry, control viscosity is 10000mPas.The slurry of milled is poured into the low level storing of roll coating system again
In tank, pressure revolution speed 50r/min is adjusted, electronic roller coating idler wheel revolving speed 70r/min is adjusted, makes electronic roller coating wheel surface in a high position
It is sufficiently infiltrated in reservoir, is stained with slurry, then will tear single-sided parting film off, expose the base load film (commercially available) of viscous layer
It is close to roller coating wheel and carries out roller coating operation.There is the film of slurry by hot wind drying tunnel or hot drying tunnel load, temperature control is 100 DEG C,
Drying removing dispersing agent, by remove dispersing agent and load there is the film of slurry solids to be orientated by one or multi-channel stack
Roll-in, the roller speed ratio for controlling each pair of roller up and down is 1.3:1, and pressure is controlled in 40MPa, is finally protected in coating surface fitting PET
Cuticula (commercially available).Experimental products are tested according to ASTM D374 standard testing with a thickness of 30 μm, according to ASTM E1461 standard testing
Thermal coefficient is up to 830W/mK.
Embodiment 6
The number of plies for weighing 1kg first is the graphene powder (N008-P) of 5~8 layers of graphene, is dispersed to waterglass
In solution, the mass ratio 6:1 of Graphene powder weight and water glass solution solute is controlled, through paste mill grinding, centre can add water
The viscosity of slurry is adjusted, control viscosity is 8000mPas.The slurry of milled is poured into the low level storage tank of roll coating system again, is adjusted
Pressure revolution speed 50r/min is saved, electronic roller coating idler wheel revolving speed 40r/min is adjusted, makes electronic roller coating wheel surface in high-order reservoir
In sufficiently infiltrate, be stained with slurry, then will tear single-sided parting film off, expose (commercially available) the abutting roller of base load film of viscous layer
It applies wheel and carries out roller coating operation.There is the film of slurry by hot wind drying tunnel or hot drying tunnel load, temperature control is 110 DEG C, and drying is de-
Except dispersing agent, by remove dispersing agent and loading has the film of slurry solids to carry out orientation roll-in by one or multi-channel stack,
Controlling each pair of roller roller speed ratio up and down is 1.2:1, and pressure is controlled in 45MPa, is finally bonded PET protection film (city in coating surface
It sells).Experimental products according to ASTM D374 standard testing with a thickness of 40 μm, can according to ASTM E1461 standard testing thermal coefficient
Up to 640W/mK.
Claims (7)
1. a kind of conduction graphite film, which is characterized in that the conduction graphite film is four-layer structure, six layer structure or seven-layer structure；Its
In, four-layer structure is successively from top to bottom release film or release paper-graphene or expanded graphite coating-acrylic compounds adhesive layer-
Release film；From top to bottom successively release film or release paper-graphene or expanded graphite coating-acrylic compounds bond six layer structure
Layer-ultra-thin PI or PEEK high temperature resistant enhances film-acrylic compounds adhesive layer-release film；Seven-layer structure from top to bottom successively release film
Or release paper-graphene or expanded graphite coating-acrylic compounds adhesive layer-ultra-thin PI or PEEK high temperature resistant enhance film-acrylic acid
Class adhesive layer-graphene or expanded graphite coating-release film or release paper；The conduction graphite film can be by following steps system
It is standby:
A, the allotment of graphene or expanded graphite dispersion liquid slurry: by graphene or expanded graphite powder be distributed to containing water-soluble or
In the solution of the molten Environment-friendlyadhesive adhesive of ethyl alcohol, control adhesive guarantees to close with the mass ratio of graphene or expanded graphite powder
It is 4:1~10:1 that suitable viscosity, which is suitable for roller coating technology, graphene or expanded graphite powder and the mass ratio of adhesive, described
Containing water-soluble or the molten Environment-friendlyadhesive adhesive of ethyl alcohol are butadiene-styrene rubber/carboxymethyl cellulose lotion, nature rubber latex, butyronitrile rubber
Latex solution, polytetrafluoroethyl-ne aqueous solution, polyvinyl alcohol water solution, acrylic acid/esters class lotion, gathers at butadiene rubber lotion
Urethane lotion or hydroxyethyl cellulose ethanol solution, the roller coating technology viscosity are 3000mPas~10000mPas；
B, multilayered structure substrate film selects: substrate film is three layers or five-layer structure, when substrate film is three-decker, on
Layer is the PET release film of 0.15~0.03mm, and centre is the propylene acids adhesive layer of 0.006~0.03mm, and lower layer is that thickness exists
The PET release layer of 0.01~0.05mm；When substrate film is five-layer structure, upper layer is the PET release film of 0.15~0.03mm, in
Between three layers be the propylene acids adhesive that two sides is coated with 0.001~0.005mm thickness 0.01~0.05mm PI or
The film of the resistance to 200 DEG C of high temperature of PEEK, the bottom are the PET release film layer of 0.01~0.05mm；
C, roller coating, drying and orientation roll-in: first in the enterprising Line Continuity roller coating allotment of the viscous layer of multilayered structure substrate film
Good graphene or expanded graphite dispersion liquid slurry, roller coating process is by adjusting pressure pump and roller speed, by graphene or swollen
Swollen graphite dispersing solution slurry is coated uniformly on substrate film；Then there is the substrate of graphene or expanded graphite coating thin roller coating
Film carries out drying and processing；One or many orientation roll-ins are carried out to film again, keep graphene or expanded graphite coating more compact close
Real, crystal grain orientation is regular；Finally ultra-thin adhesive layer or surface protection film are enclosed in coating surface.
2. the preparation method of conduction graphite film described in claim 1 carries out as steps described below:
A, the allotment of graphene or expanded graphite dispersion liquid slurry: by graphene or expanded graphite powder be distributed to containing water-soluble or
In the solution of the molten Environment-friendlyadhesive adhesive of ethyl alcohol, control adhesive guarantees to close with the mass ratio of graphene or expanded graphite powder
It is 4:1~10:1 that suitable viscosity, which is suitable for roller coating technology, graphene or expanded graphite powder and the mass ratio of adhesive, described
Containing water-soluble or the molten Environment-friendlyadhesive adhesive of ethyl alcohol are butadiene-styrene rubber/carboxymethyl cellulose lotion, nature rubber latex, butyronitrile rubber
Latex solution, polytetrafluoroethyl-ne aqueous solution, polyvinyl alcohol water solution, acrylic acid/esters class lotion, gathers at butadiene rubber lotion
Urethane lotion or hydroxyethyl cellulose ethanol solution, the roller coating technology viscosity are 3000mPas~10000mPas；
B, multilayered structure substrate film selects: substrate film is three layers or five-layer structure, when substrate film is three-decker, on
Layer is the PET release film of 0.15~0.03mm, and centre is the propylene acids adhesive layer of 0.006~0.03mm, and lower layer is that thickness exists
The PET release layer of 0.01~0.05mm；When substrate film is five-layer structure, upper layer is the PET release film of 0.15~0.03mm, in
Between three layers be the propylene acids adhesive that two sides is coated with 0.001~0.005mm thickness 0.01~0.05mm PI or
The film of the resistance to 200 DEG C of high temperature of PEEK, the bottom are the PET release film layer of 0.01~0.05mm；
C, roller coating, drying and orientation rolling process: roller coating technology is connected on the viscous layer using multilayered structure substrate film
The operation of continuous property roller coating deployed graphene or expanded graphite dispersion liquid slurry, roller coating process is by adjusting pressure pump and roller
Graphene or expanded graphite dispersion liquid slurry are coated uniformly on substrate film by revolving speed；Wherein, drying process is that have roller coating
The substrate film of graphene or expanded graphite coating carries out drying and processing, then carries out one or many orientation roll-ins to film,
Keep graphene or expanded graphite coating more compact closely knit, crystal grain orientation is regular；Ultra-thin adhesive layer or table are enclosed in coating surface again
Surface protective film.
3. the preparation method of conduction graphite film according to claim 2, which is characterized in that the graphene be single layer or
Multilayer chip structure；The expanded graphite is the worm laminated structure graphite that expansion multiple is greater than 100 times.
4. the preparation method of conduction graphite film according to claim 2, which is characterized in that Graphene powder weight and natural
The mass ratio 9:1 of rubber latex solute.
5. the preparation method of conduction graphite film according to claim 2, which is characterized in that Graphene powder weight and poly- second
The mass ratio 9.5:1 of enol aqueous solute.
6. the preparation method of conduction graphite film according to claim 2, which is characterized in that expanded graphite powder quality and fourth
The mass ratio 8.5:1 of nitrile rubber lotion solute.
7. the preparation method of conduction graphite film according to claim 2, which is characterized in that the drying process is removal
Solvent, dry using heated-air drying or hot drying tunnel, temperature is 90~120 DEG C；The orientation roll-in is coated after drying
There is the substrate film of graphene or expanded graphite coating under upper and lower each pair of roller differential roller speed ratio by 2~5 roll-ins, up and down
Each pair of roller roller Transmission Ratio Control is controlled in 1.5:1~1:1, pressure in 20~50MPa, and thickness control keeps its attached at 10~80 μm
In on the viscous layer of substrate film；The graphene or expanded graphite coating surface protective film uses the release film of environment-friendly type
Or release paper.
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| CN105788879B (en) * | 2016-04-27 | 2019-05-03 | 东华大学 | A kind of graphene film and its continuous preparation method |
| CN105964522B (en) * | 2016-05-05 | 2019-10-11 | 中国科学院长春应用化学研究所 | A kind of preparation method of graphene heat conducting film |
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Application publication date: 20151202 Assignee: Shanghai Li Sheng Nano Technology Co., Ltd. Assignor: Shanghai Co., Ltd of Li Wusheng enterprise group Contract record no.: X2019310000016 Denomination of invention: Method for efficiently and continuously preparing heat-conducting graphite film on large area Granted publication date: 20190621 License type: Exclusive License Record date: 20191015 |