CN109852274A - A kind of graphene conductive adhesive film and its preparation process - Google Patents
A kind of graphene conductive adhesive film and its preparation process Download PDFInfo
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- CN109852274A CN109852274A CN201811632231.9A CN201811632231A CN109852274A CN 109852274 A CN109852274 A CN 109852274A CN 201811632231 A CN201811632231 A CN 201811632231A CN 109852274 A CN109852274 A CN 109852274A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 85
- 239000002313 adhesive film Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000010410 layer Substances 0.000 claims abstract description 54
- 239000002346 layers by function Substances 0.000 claims abstract description 44
- 239000000853 adhesive Substances 0.000 claims abstract description 18
- 230000001070 adhesive effect Effects 0.000 claims abstract description 18
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000011241 protective layer Substances 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 229920006254 polymer film Polymers 0.000 claims abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 51
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 34
- 238000001556 precipitation Methods 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000011787 zinc oxide Substances 0.000 claims description 17
- 238000000643 oven drying Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- -1 release glue-line Substances 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 6
- 229920005749 polyurethane resin Polymers 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 229920001568 phenolic resin Polymers 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- 229920006269 PPS film Polymers 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 239000004645 polyester resin Substances 0.000 claims description 4
- 229920001225 polyester resin Polymers 0.000 claims description 4
- 239000009719 polyimide resin Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000012767 functional filler Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 claims 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 claims 1
- 229920002125 Sokalan® Polymers 0.000 claims 1
- 239000004584 polyacrylic acid Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 238000010276 construction Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 44
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 33
- 238000002156 mixing Methods 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
- 239000000126 substance Substances 0.000 description 10
- 229910052582 BN Inorganic materials 0.000 description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000012948 isocyanate Substances 0.000 description 7
- 150000002513 isocyanates Chemical class 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- 239000004925 Acrylic resin Substances 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 239000007822 coupling agent Substances 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- SHPBBNULESVQRH-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[Zr+4] Chemical compound [O-2].[O-2].[Ti+4].[Zr+4] SHPBBNULESVQRH-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000002633 protecting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
The present invention provides a kind of graphene conductive adhesive film, from bottom to up successively includes carrier film layer, release glue-line, graphene functional layer and release protective layer；The carrier film layer is high molecular polymer film layer, with a thickness of 25-100 μm；The release glue-line is made of adhesive main body and the functional stuffing being distributed in adhesive main body, with a thickness of 5~50 μm；The graphene functional layer is the composite material of graphene and macromolecular adhesive composition, with a thickness of 2~50 μm；The release protective film layer is with a thickness of 12-200 μm.Graphene conductive adhesive film of the invention, overall construction design is succinct, and film thickness obtained can be made flexible ultra-thin；Manufacturing process of the invention is easy to accomplish, by conventional dispersion, is coated and dried technique and can be realized, facilitates commercial introduction application.
Description
Technical field
The invention belongs to Heat Conduction Material technical fields, and in particular to a kind of graphene conductive adhesive film and its preparation process.
Background technique
Heat conduction and heat radiation material is material indispensable in electronic product, is widely used in computer and its periphery at present
In equipment, communication product and consumer electrical product, with the sustainable growth of consumer electrical product demand and intelligent requirements
It gradually rises, Heat Conduction Material is put forward higher requirements.
In the electronic products such as smart phone, tablet computer, need using a large amount of thermally conductive/cooling fin and glue film.At present
Thermally conductive/the heat sink material used in the market is based on heat-conducting silicone grease, cooling fin, it is difficult to the requirement for adapting to " light, thin, soft, tough ", because
This is highly desirable to the use demand for developing the new Heat Conduction Material of one kind to meet electronic product.
Summary of the invention:
It is an object of the present invention to provide a kind of graphene conductive adhesive films, to solve the problems, such as the relevant art in existing, have light
Matter, high thermal conductivity/thermal diffusivity, thickness is thin, light release feature convenient to use.
Another object of the present invention is to provide a kind of preparation process of graphene conductive adhesive film, the process step letters
Single, quality stabilization, high production efficiency, are suitble to large-scale industrial production.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of graphene conductive adhesive film, from bottom to up successively include carrier film layer, release glue-line, graphene functional layer and
Release protective layer；
The carrier film layer is high molecular polymer film layer, with a thickness of 25-100 μm；
The release glue-line is made of adhesive main body and the functional stuffing that is distributed in adhesive main body, with a thickness of 5~
50μm；
The graphene functional layer is the composite material of graphene and macromolecular adhesive composition, with a thickness of 2~50 μm；
The release protective film layer is with a thickness of 12-200 μm.
In preferred embodiment, the carrier film layer is the one or more of of PET, PI, PBT, PPS film
Modified film.Carrier film layer plays the role of carrying to release glue-line and graphene functional layer.
In preferred embodiment, the release glue-line include epoxy resin, polyacrylic resin, modified rubber,
The mixture of one or more of phenolic resin, organic siliconresin, polyester resin, polyurethane resin and it is scattered in mixture
Thermal conductivity filler in matrix, specifically includes each component of following parts by weight: 10~50 parts of resin, 3~20 parts of curing agent, thermally conductive
10~60 parts of particle, 5~30 parts of solvent, 0.5~2 part of activating agent.Have and lead on an equal basis for compound one layer in the conductive adhesive film of this programme
The release glue-line of thermal energy power, particularly convenient terminal electronic product uses, convenient for the replacement of conductive adhesive film.The curing agent is methyl
Any one or a few mixture in tetrahydro acid anhydrides, isocyanates or modified amine.
In preferred embodiment, the conductive particle is aluminium oxide, boron nitride, zinc oxide or titanium dioxide silicon grain
Son.The diameter of the conductive particle is 1-10 μm, and such release glue-line has better heating conduction.
In preferred embodiment, the release protective film layer be PET release film, PP release film, PBT release film or
One of release paper.By the way that a leafing type protective film layer is arranged in graphene functional layer, so that graphene conductive adhesive film
Protecting effect is more preferable.
In preferred embodiment, the graphene functional layer is by adhesive main body and is distributed in adhesive main body
Functional stuffing composition, the adhesive main body is modified epoxy, polyacrylic resin, polyimide resin, modified rubber
The mixture of one or more of glue, phenolic resin, organic siliconresin, polyester resin, polyurethane resin, carbamide resin.This
Compound graphene functional layer is used in scheme, and there is excellent thermally conductive, thermal diffusivity, it is ultralight, ultra-thin to have shielding properties.
In preferred embodiment, the functional filler is that graphene powder is answered with what other heat fillings adulterated
Condensation material.
In preferred embodiment, the graphene functional layer specifically includes each component of following parts by weight: gluing
10~50 parts of agent main body, 0.5~20 part of curing agent, 0.5~10 part of graphene, 0.5~20 part of nano zine oxide, nanometer titanium dioxide
Zirconium 0.5~20,0.5~20 part of nano aluminium oxide, 0.1~1 part of yttrium oxide, 5~30 parts of solvent, 0.5~2 part of activating agent.It is described
Curing agent is the mixture of one of isocyanates or methyl anhydride or any component.
The present invention also provides a kind of preparation methods of above-mentioned graphene conductive adhesive film, comprising the following steps:
S1, it is coated with thermally conductive release glue-line on a carrier film, 0.5~4m/min of stroke is coated with, through oven drying precipitation, thickness
It is 5-50 μm；
S2, it is coated with graphene functional layer on A1 layer, is coated with 2~6m/min of stroke, when oven drying precipitation, with a thickness of 2-
50μm；
A leafing type protective film is pressed on S3, the A2 layer after precipitation, with a thickness of 12-200 μm, winding.
It is furthermore preferred that setting temperature gradient is 40~160 DEG C when dry in baking oven in the step S1；The step S2
When dry in middle baking oven, setting temperature gradient is 40~160 DEG C.
Conductive adhesive film of the invention uses graphene functional layer, has excellent thermally conductive, thermal diffusivity, ultralight, ultra-thin to have
Shielding properties；The compound one layer release glue-line for having the same capacity of heat transmission under functional layer, particularly convenient terminal use, convenient for more
It changes；Overall construction design is succinct, and flexibility is good, enables to film thickness obtained flexible ultra-thin；With excellent caking property
Can, weather-proof, endurance has the intensity of higher machinery；With excellent thermally conductive and heat dissipation performance, thermal coefficient is 0.8~3W；It can
To meet the flexibility design requirement of flexible electronic product for electronic products such as mobile phone, computers.Conductive adhesive film of the invention
Manufacturing technology steps it is simple, by conventional dispersion, be coated and dried technique and can be realized, easy to control, quality is stablized, side
Just industrialized production.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of graphene conductive adhesive film of the invention；
Appended drawing reference: 1- carrier film layer, the release glue-line of 2-, 3- graphene functional layer, 4- release protective layer.
Specific embodiment
The preferred embodiment of the present invention presented below, to help the present invention is further understood.Those skilled in the art answer
It solves, the explanation of the embodiment of the present invention is merely exemplary, the scheme being not meant to limit the present invention.
Embodiment 1
Referring to attached drawing 1, graphene conductive adhesive film in the present embodiment is four layers of superthin structure flexible, from top to bottom according to
Secondary includes: carrier film layer 1, the release glue-line 2 being coated on carrier film layer 1, the graphene function being coated on release glue-line 2
Ergosphere 3 and the release protective layer 4 being pressed in graphene functional layer 3, thermal coefficient 1.7W/mk.
Carrier film layer 1 plays the role of carrying to release glue-line 2 and graphene functional layer 3, is high molecular polymer film
Layer, it is PET film in the present embodiment, with a thickness of 25 μm.
Release glue-line 2 has the glue-line of thermally conductive function, 5 μm of thickness, fills for rubber modified epoxy resin adhesive thermally conductive
Particle is combined, and specifically includes following component according to parts by weight: 20 parts of nitrile rubber, 25 parts of epoxy resin, and 3 parts of modified amine,
30 parts of aluminium oxide, 2 parts of boron nitride, 4 parts of zinc oxide, silica 1 part, 0.6 part of Silane coupling agent KH550, ethyl acetate 30
Part.Above-mentioned substance is dispersed mixing and is coated on substrate, and release glue-line 2 is formed after baking oven precipitation rapid curing.It is wherein silane coupled
Agent KH550 is activating agent, and ethyl acetate is solvent, and aluminium oxide, boron nitride, zinc oxide and silica are that diameter is 1-10 μm
Conductive particle.
Graphene functional layer 3 has thermally conductive/heat dissipation and adhesive function, and graphene functional layer 3 is acrylic acid in the present embodiment
The adhesive main body filled graphite alkene Heat Conduction Material of resin is combined, with a thickness of 15 μm.Graphene functional layer specifically include with
The each component of lower parts by weight: 45 parts of acrylic resin, 4 parts of graphene, 6 parts of rutile type nano zinc oxide, nano zirconium dioxide
12 parts, 0.1 part of yttrium oxide, 8 parts of nano aluminium oxide, 30 parts of ethyl acetate, 0.5 part of coupling agent KH560,5 parts of isocyanates；On
It states substance to be placed in mixing machine, forms graphene functional layer 3 after mixing with high speed dispersion.
Release protective film layer 4 is PET release film, with a thickness of 20 μm.
Graphene conductive adhesive film in the present embodiment is four layers of superthin structure, has a good flexibility, heat-resisting, resistance toization,
Weather resistance, have good thermally conductive/heat dissipation performance, have electromagnetic wave shielding, the compound release very convenient use of glue-line, very well
Ground meets the demand of electronic product industry.
The manufacturing process of graphene conductive adhesive film in the present embodiment specifically includes the following steps:
Greasy dirt and foreign matter on S1, removing carrier thin film volume inner face, and it is coated with release glue-line on it, it is coated with stroke
0.5m/min, through oven drying precipitation, setting temperature gradient is 40~100 DEG C in baking oven；
Graphene functional layer is coated on S2, release glue-line, coating stroke 2m/min is set in baking oven through oven drying precipitation
Setting temperature gradient is 40~120 DEG C；
Release protective layer is pressed on S3, graphene functional layer, is wound；
S4, it cuts, stores.
The processes such as used removing foreign matter, coating, precipitation are already mature in the prior art in above-mentioned manufacturing process
Common technology, do not repeat.
Embodiment 2
Graphene conductive adhesive film in the present embodiment, it is in the same manner as in Example 1, from top to bottom successively include four-layer structure:
Carrier film layer, the release glue-line being coated on carrier film layer, the graphene functional layer and pressure being coated on release glue-line
Together in the release protective layer in graphene functional layer, thermal coefficient 1.9W/mk.
Carrier film layer is PI modified film in the present embodiment, with a thickness of 50 μm.Release bondline thickness is 20 μm, according to weight
Amount part specifically includes following component: 10 parts of phenolic resin, 15 parts of epoxy resin, and 5 parts of methyl tetra-hydrogen anhydride, 25 parts of aluminium oxide, nitrogen
Change 5 parts of boron, 3 parts of zinc oxide, 2 parts of silica, 1 part of Silane coupling agent KH550,26 parts of ethyl acetate.Above-mentioned substance is dispersed
Mixing is coated on substrate, forms release glue-line after baking oven precipitation rapid curing.Conductive particle aluminium oxide, boron nitride, zinc oxide and
The diameter of silicon dioxide granule is 1-10 μm.
Graphene functional layer specifically includes each component of following parts by weight: organosilicon tree with a thickness of 20 μm in the present embodiment
25 parts of rouge, 15 parts of polyurethane resin, 6 parts of graphene, 5 parts of rutile type nano zinc oxide, 8 parts of nano zirconium dioxide, yttrium oxide
0.6 part, 10 parts of nano aluminium oxide, 28 parts of ethyl acetate, 0.8 part of coupling agent KH560,8 parts of isocyanates；Above-mentioned substance is placed in
In mixing machine, graphene functional layer is formed after mixing with high speed dispersion.
Release protective film layer is PP release film, with a thickness of 50 μm.
The manufacturing process of graphene conductive adhesive film in the present embodiment is roughly the same with embodiment 1, and specific difference is:
The coating stroke 2m/min of S1, the release glue-line of coating, through oven drying precipitation, setting temperature gradient is 60 in baking oven
~120 DEG C；
Graphene functional layer is coated on S2, release glue-line, coating stroke 5m/min is set in baking oven through oven drying precipitation
Setting temperature gradient is 60~120 DEG C.
Embodiment 3
Graphene conductive adhesive film in the present embodiment, it is in the same manner as in Example 1, from top to bottom successively include four-layer structure:
Carrier film layer, the release glue-line being coated on carrier film layer, the graphene functional layer and pressure being coated on release glue-line
Together in the release protective layer in graphene functional layer, thermal coefficient 2.2W/mk.
Carrier film layer is PBT film in the present embodiment, with a thickness of 100 μm.Release bondline thickness is 50 μm, according to weight
Part specifically includes following component: 20 parts of polyurethane resin, 25 parts of organic siliconresin, 20 parts of isocyanates, 40 parts of aluminium oxide, nitrogenizing
10 parts of boron, 5 parts of zinc oxide, 5 parts of silica, 2 parts of Silane coupling agent KH550,30 parts of ethyl acetate.Above-mentioned substance is dispersed
Mixing is coated on substrate, forms release glue-line after baking oven precipitation rapid curing.Conductive particle aluminium oxide, boron nitride, zinc oxide and
The diameter of silicon dioxide granule is 1-10 μm.
Graphene functional layer specifically includes each component of following parts by weight: polyimides with a thickness of 50 μm in the present embodiment
25 parts of resin, 25 parts of carbamide resin, 10 parts of graphene, 15 parts of rutile type nano zinc oxide, 10 parts of nano zirconium dioxide, oxidation
01 part of yttrium, 15 parts of nano aluminium oxide, 30 parts of ethyl acetate, 2 parts of coupling agent KH560,0.7 part of isocyanates；Above-mentioned substance is placed in
In mixing machine, graphene functional layer is formed after mixing with high speed dispersion.
Release protective film layer is PP release film, with a thickness of 100 μm.
The manufacturing process of graphene conductive adhesive film in the present embodiment is roughly the same with embodiment 1, and specific difference is:
The coating stroke 3m/min of S1, the release glue-line of coating, through oven drying precipitation, setting temperature gradient is 80 in baking oven
~160 DEG C；
Graphene functional layer is coated on S2, release glue-line, coating stroke 6m/min is set in baking oven through oven drying precipitation
Setting temperature gradient is 80~160 DEG C.
Embodiment 4
Graphene conductive adhesive film in the present embodiment, it is in the same manner as in Example 1, from top to bottom successively include four-layer structure:
Carrier film layer, the release glue-line being coated on carrier film layer, the graphene functional layer and pressure being coated on release glue-line
Together in the release protective layer in graphene functional layer, thermal coefficient 2.5W/mk.
Carrier film layer is PPS film in the present embodiment, with a thickness of 80 μm.Release bondline thickness is 40 μm, according to weight
Part specifically includes following component: 15 parts of phenolic resin, 15 parts of epoxy resin, 15 parts of polyacrylic resin, 15 parts of modified amine, aoxidizing
20 parts of aluminium, 15 parts of boron nitride, 5 parts of zinc oxide, 5 parts of silica, 2 parts of Silane coupling agent KH550,20 parts of ethyl acetate.It is above-mentioned
Substance is dispersed mixing and is coated on substrate, forms release glue-line after baking oven precipitation rapid curing.Conductive particle aluminium oxide, nitridation
The diameter of boron, zinc oxide and silicon dioxide granule is 1-10 μm.
Graphene functional layer specifically includes each component of following parts by weight: modified rubber with a thickness of 40 μm in the present embodiment
15 parts, 15 parts of polyimide resin, 10 parts of polyester resin, 8 parts of graphene, 10 parts of rutile type nano zinc oxide, nano-silica
Change 16 parts of zirconium, 1 part of yttrium oxide, 16 parts of nano aluminium oxide, 20 parts of ethyl acetate, 2 parts of coupling agent KH560,18 parts of methyl anhydride；
Above-mentioned substance is placed in mixing machine, and graphene functional layer is formed after mixing with high speed dispersion.
Release protective film layer is PP release film and PBT release film composite layer, with a thickness of 150 μm.
The manufacturing process of graphene conductive adhesive film in the present embodiment is roughly the same with embodiment 1, and specific difference is:
The coating stroke 4m/min of S1, the release glue-line of coating, through oven drying precipitation, setting temperature gradient is 80 in baking oven
~100 DEG C；
Graphene functional layer is coated on S2, release glue-line, coating stroke 6m/min is set in baking oven through oven drying precipitation
Setting temperature gradient is 80~100 DEG C.
Embodiment 5
Graphene conductive adhesive film in the present embodiment, it is in the same manner as in Example 1, from top to bottom successively include four-layer structure:
Carrier film layer, the release glue-line being coated on carrier film layer, the graphene functional layer and pressure being coated on release glue-line
Together in the release protective layer in graphene functional layer, thermal coefficient 0.9W/mk.
Carrier film layer is PBT and PPS film composite in the present embodiment, with a thickness of 100 μm.Release bondline thickness is 50
μm, following component is specifically included according to parts by weight: 5 parts of modified rubber, 5 parts of polyacrylic resin, 5 parts of polyurethane resin, methyl
15 parts of mixture of tetrahydro acid anhydrides and isocyanate weight ratio 14:1,5 parts of aluminium oxide, 2 parts of boron nitride, 2 parts of zinc oxide, titanium dioxide
1 part of silicon, 0.5 part of Silane coupling agent KH550,5 parts of ethyl acetate.Above-mentioned substance is dispersed mixing and is coated on substrate, baking oven precipitation
Release glue-line is formed after rapid curing.Conductive particle aluminium oxide, boron nitride, zinc oxide and silicon dioxide granule diameter be 1-10
μm。
Graphene functional layer specifically includes each component of following parts by weight: modified epoxy with a thickness of 50 μm in the present embodiment
5 parts of resin, 5 parts of polyimide resin, 0.5 part of graphene, 0.5 part of rutile type nano zinc oxide, nano zirconium dioxide 0.5
Part, 0.3 part of yttrium oxide, 0.5 part of nano aluminium oxide, 5 parts of ethyl acetate, 0.5 part of coupling agent KH560,0.5 part of methyl anhydride；On
It states substance to be placed in mixing machine, forms graphene functional layer after mixing with high speed dispersion.
Release protective film layer is PBT release film, with a thickness of 15 μm.
The manufacturing process of graphene conductive adhesive film in the present embodiment is roughly the same with embodiment 1, and specific difference is:
The coating stroke 0.5m/min of S1, the release glue-line of coating, through oven drying precipitation, setting temperature gradient is in baking oven
100~160 DEG C；
Graphene functional layer is coated on S2, release glue-line, coating stroke 2m/min is set in baking oven through oven drying precipitation
Setting temperature gradient is 100~160 DEG C.
Finally it should be noted that above embodiments are merely to illustrate the technical solution of the application rather than to its protection scope
Limitation, although the application is described in detail referring to above-described embodiment, the those of ordinary skill in the field should
Understand: those skilled in the art read the specific embodiment of application can still be carried out after the application various changes, modification or
Equivalent replacement, but the above change, modification or equivalent replacement, in the application wait authorize or the claim of issued for approval protection model
Within enclosing.
Claims (9)
1. a kind of graphene conductive adhesive film, which is characterized in that from bottom to up successively include carrier film layer, release glue-line, graphite
Olefinic functionality layer and release protective layer；
The carrier film layer is high molecular polymer film layer, with a thickness of 25-100 μm；
The release glue-line is made of adhesive main body and the functional stuffing being distributed in adhesive main body, with a thickness of 5~50 μm；
The graphene functional layer is the composite material of graphene and macromolecular adhesive composition, with a thickness of 2~50 μm；
The release protective film layer is with a thickness of 12-200 μm.
2. graphene conductive adhesive film according to claim 1, which is characterized in that the carrier film layer be PET, PI,
One or more of modified films of PBT, PPS film.
3. graphene conductive adhesive film according to claim 1, which is characterized in that the release glue-line includes following parts by weight
Each component: 10~50 parts of resin, 3~20 parts of curing agent, 10~60 parts of conductive particle, 5~30 parts of solvent, activating agent 0.5~2
Part.
4. graphene conductive adhesive film according to claim 3, which is characterized in that the conductive particle is aluminium oxide, nitridation
Boron, zinc oxide or silicon dioxide granule.
5. graphene conductive adhesive film according to claim 1, which is characterized in that the release protective film layer is that PET is release
One of film, PP release film, PBT release film or release paper.
6. graphene conductive adhesive film according to claim 1, which is characterized in that the graphene functional layer is by adhesive master
Body and the functional stuffing being distributed in adhesive main body form, and the adhesive main body is modified epoxy, polyacrylic acid tree
Rouge, polyimide resin, modified rubber, phenolic resin, organic siliconresin, polyester resin, polyurethane resin, in carbamide resin
One or more of mixtures.
7. graphene conductive adhesive film according to claim 6, which is characterized in that the functional filler is graphene powder
With the composite material of other heat fillings doping.
8. the preparation method of graphene conductive adhesive film described in -7 any one according to claim 1, which is characterized in that including with
Lower step:
S1, it is coated with thermally conductive release glue-line on a carrier film, 0.5~4m/min of stroke is coated with, through oven drying precipitation；
S2, it is coated with graphene functional layer on A1 layer, is coated with 2~6m/min of stroke, temperature gradient, oven drying precipitation are set
When；
A leafing type protective film is pressed on S3, the A2 layer after precipitation, is wound.
9. the preparation method of graphene conductive adhesive film according to claim 8, which is characterized in that in the step S1, dry
Setting temperature gradient is 40~160 DEG C when dry in case；When dry in baking oven in the step S2, setting temperature gradient is 40~
160℃。
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| CN113956806A (en) * | 2021-12-07 | 2022-01-21 | 江苏穗实科技有限公司 | Preparation method of flexible composite material for MiniLED |
| WO2022124005A1 (en) * | 2020-12-11 | 2022-06-16 | 富士フイルム株式会社 | Curable composition, thermally conductive material, thermally conductive sheet, and device with thermally conductive layer |
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