CN105869770B - A kind of mechanical stripping prepares graphene conductive slurry and preparation method thereof - Google Patents
A kind of mechanical stripping prepares graphene conductive slurry and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
Abstract
Graphene conductive slurry and preparation method thereof is prepared the invention discloses a kind of mechanical stripping, the slurry constituent is as follows：Graphene suspension 50 80%, conductive filler 20 50%, binding agent 5 15%, auxiliary packing 0 10%, functional additive 0 5%, highly conductive polymeric dispersant 0 5%.Its preparation method comprises the following steps：Intercalation processing first will be carried out to graphene in organic solvent with high molecular surfactant, then it is by mechanically pulling off and prepares graphene suspension, then filtration treatment is carried out to the suspension after mechanical stripping, is eventually adding conductive filler, binding agent, auxiliary packing, functional additive and stirs and produce graphene conductive slurry.The present invention carries out intercalation processing using surfactant, to protect graphene-structured complete, and directly prepares graphene conductive slurry using one-step method.Simplify and first prepare the complex techniques process that graphene prepares electrocondution slurry again, the electric property of graphene conductive slurry and the dispersiveness of slurry and stability are improved again.
Description
Technical field
The present invention relates to the method for preparing graphene conductive slurry using mechanical stripping in organic solvent.
Background technology
2004, the Univ Manchester UK strong K Hai Mu of peace moral were taught and Constantine Nuo Woxiao love professors
First passage adhesive tape stripping means is prepared for single-layer graphene, and subsequent graphene becomes the research heat of material supply section educational circles of the world
Point.By constantly studying it discovery, graphene has excellent mechanics, calorifics, electric property and optical property, at room temperature its
Electron mobility is up to 15000 cm2/Vs, and the movement velocity of electronics has reached the 1/300 of the light velocity, and resistivity only about 10-6
Ω cm are lower than copper or silver.Compared with conventional conductive slurry, graphene conductive slurry has more preferable electric property, extensively
Applied to fields such as microelectronic component, solar cell, chemical cell, LED.
At present, preparing the method for graphene mainly has Physical and chemical method.Physical is mainly the thing by storeroom
The graphene with intrinsic property is prepared in reason effect, and it is more completely chemical constitution, material that graphene prepared by this method, which has,
Material performance will not be destroyed, but obtained graphene quality is unstable, including mechanical stripping method, arc discharge method, ultrasonic method etc..
Chemical method is mainly logical chemical reaction and prepares graphene, and graphene quality prepared by the method is relatively stable, but chemical reaction process
The intrinsic structure of middle graphene may be destroyed, and caused the performance of graphene and reduced.Graphite is such as prepared using oxidation-reduction method
In alkene materials process, oxy radical destroys the sp2 hybridized orbits in graphene, forms sp3 hybridized orbits, greatly reduces
The electric conductivity of graphene.Chemical method mainly has organic synthesis method, chemical vapour deposition technique, oxidation-reduction method etc..Pass through
Prolonged research, the method for preparing graphene is more and more, and technology is also gradually improved, and realizes large-scale production, but
But it is rarely reported on application of the graphene in electrocondution slurry.
Invention herein carries out intercalation processing to high molecular surfactant to graphite first, then uses in organic solvent
The method of mechanical stripping is peeled off to the graphite after processing, is then handled suspension, directly prepares graphene conductive
Slurry.Although on preparing the patent of graphene conductive slurry it has been reported that still preparing graphene conductive slurry using one-step method
The patent of material is not yet reported.Patent 201510239652.5 is reported carries out intercalation processing using inorganic strong oxidizer to graphite,
Then graphene is prepared for by ultrasonic method.This method handles the chemical constitution for being easily destroyed graphite using strong oxidizer, makes
Sp2 hybridized orbits are reduced, and cause the hydraulic performance decline of graphene, and the present invention is carried out at intercalation using organic polymer to graphite
Reason, is conducive to protecting the chemical constitution of graphene.Patent 201510713784.7 is entered using high molecular surfactant to graphite
Row intercalation processing, is then by mechanically pulling off and is prepared for graphene, and by adjusting the hydrophilic parent of high molecular surfactant
Oily equilibrium valve（HLB）To adjust the compatibility between surfactant and different solvents, so as to improve mechanical stripping efficiency.But should
Scheme mainly studies the preparation of surfactant, and graphene conductive slurry is not studied.Patent 201410828734.9
Propose and adsorption treatment is carried out to graphenic surface using inorganic dispersant, to improve easy hair of the graphene in electrocondution slurry
The problem of raw reunion.Although the reunion between graphene can be reduced to graphene progress processing using inorganic dispersant,
Its uniformity and stability problem can not still be solved.The present invention prepares graphene using high molecular surfactant, directly obtains
There must be the suspension of preferable dispersive property, then directly carry out the preparation of electrocondution slurry, simplify first to prepare and made after graphene
Standby graphene conductive slurry technical process.And the later stage adds point that highly conductive polymer further improves graphene conductive slurry
Dissipate property and stability.
The content of the invention
, should it is a primary object of the present invention to provide a kind of mechanical stripping to prepare graphene conductive slurry and preparation method thereof
Mainly the intercalation processing including graphite, the preparation of graphene suspension, graphene conductive slurry prepare three processes to method.Using
High molecular surfactant carries out intercalation processing to graphite, to improve mechanical stripping efficiency, and protects graphene result in machinery
It is not destroyed during stripping.Then filler, functional additive etc. are added in the suspension after being filtered through copper mesh and prepares stone
Black alkene electrocondution slurry.Further graphene conductive slurry of the protection as obtained by prepared by preparation method of the present invention of the invention.
To realize that above-mentioned one-step method prepares graphene conductive slurry, this technical scheme comprises the following steps：
A is carried out after intercalation processing by high molecular surfactant to graphite, by mechanical stripping and filter process system
The more uniform graphene suspension of standby granular size.
A kind of mechanical strippings of B prepare the percentage composition of graphene conductive slurry：Graphene suspension 50-80%, it is conductive
Filler 20-50%, binding agent 5-15%, auxiliary packing 0-10%, functional additive 0-5%, highly conductive polymeric dispersant 0-5%.
According to step A, tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate, dodecyl will be selected from
In at least one of tetramethyl guanidine carbonate and cetyl tetramethylammonium guanidine carbonate surfactant solution organic solvent.
Preferably, the mass percent of surfactant is 5-20%.
Preferably, organic solvent is selected from butyl acetate, diethyl carbonate, DBE, ethyl carbitol acetate, methyl ethyl carbonate
Ester, butyl carbitol acetate, butyl cellosolve acetate, propene carbonate, DMSO, dimethyl succinate, propylene glycol monomethyl ether
Any of acetate, NMP, dimethylbenzene, dibutyl phthalate, dimethyl carbonate and diphenyl carbonate are two or more
Combination.
According to step A, graphite is added in the organic solution dissolved with surfactant.
Preferably, graphite soaks 30-60min in organic solution, fully to complete intercalation process.
According to step A, graphite-organic solution mixture is carried out using at least one of ball milling, Ball-stirring mill method, ultrasound
Mechanical stripping.
According to step A, copper mesh of the graphite-organic solution after mechanical stripping through 300 mesh is subjected to filtration treatment, filtering is taken
Suspension afterwards is standby.
According to step B, it is preferred that graphene homemade graphene suspension in step A.
According to step B, further, conductive filler be selected from copper powder, silver powder, aluminium powder or aluminium alloy, nickel powder, CNT,
Conductive carbon fibre, acetylene black, conductive titanium dioxide, conductive ferrorphosphorus powder, any of or two or more combinations.
According to step B, further, binding agent, which is selected from, includes phenolic resin, epoxy resin, polyester resin, vinyl tree
Any of fat, polyurethane resin, polyketone resin, ethyl cellulose or two or more combinations.
According to step B, further, auxiliary packing includes appointing in glass dust, SnO2, ZnO, Al2O3, TiO2, SiO2
What one or two kinds of combination of the above.
According to step B, further, selection VTES is as coupling agent, and BYK-161 is used as advection
Agent, ethanol is used as defoamer and sagging inhibitor.
According to step B, further, selection sodium carboxymethylcellulose is dispersant, to improve slurry dispersiveness and stably
Property.
According to step B, the preparation process of graphene conductive slurry is as follows：
The graphene suspension and organic adhesive of certain mass are weighed according to the mass percent of graphene conductive slurry
Agent, at 60-80 DEG C, by stirring in binder solution graphene suspension.
Conductive filler, auxiliary packing, functional additive, the dispersant of certain mass are weighed according to slurry percentage composition,
It is stirred with being dissolved with the graphene suspension of adhesive and mixed.
Preferably, the stirring of slurry is stirred under vacuum at 30-60 DEG C is well mixed, and produces graphene conductive slurry.
The present invention has advantage compared with other methods for preparing slurry：
It is of the invention direct using graphite as raw material, graphene conductive slurry is directly prepared using one-step method.It is with having reported
Graphene conductive slurry preparation method is compared, and this method eliminates and first prepares graphene, then obtained graphene is prepared into led
The tedious steps of plasma-based material.
Prepare graphene suspension in the process, intercalation is carried out with high molecular surfactant, it is to avoid use strong oxygen
Agent carries out the problem of intercalation destroys intrinsic graphene chemical constitution, is conducive to protecting graphene-structured, improves the conduction of slurry
Performance.
The present invention uses highly conductive polymers carboxymethylcellulo,e sodium as the dispersant of slurry, and the patent reported makes
There is more preferable dispersion effect as dispersant with inorganic carbon dust, the uniformly dispersed of graphene conductive slurry can be preferably improved
And stability.
Brief description of the drawings
Fig. 1 prepares the process chart of conductive graphene for mechanical stripping in the present invention.
Specific embodiment
The technology of the present invention is understood for convenience, illustrates to describe to technical scheme in detail below in conjunction with the accompanying drawings.The present invention with
Graphite is raw material, and in organic solvent to preparing graphene suspension using mechanical stripping method after graphite progress intercalation processing,
Graphene conductive slurry is prepared by adding highly conductive polymeric dispersant on this basis, to improve the electric conductivity of slurry, divide
Dissipate property and stability.According to accompanying drawing 1, the technical scheme mainly includes at four steps, the intercalation processing of S1 graphite, S2 intercalations
Filtering prepares graphene suspension after the mechanical stripping of graphite after reason, S3 mechanical strippings, and S4 is prepared by graphene suspension
Electrocondution slurry.
Step S1, at 50-80 DEG C, by the 10-40g tetramethyl ammonium hydrogen carbonates weighed, tetraethyl ammonium hydrogen carbonate, the tetrabutyl
A kind of surfactant in ammonium hydrogen carbonate be dissolved under magnetic stirring 160-190g butyl acetates, diethyl carbonate, DBE,
Ethyl carbitol acetate, methyl ethyl carbonate, butyl carbitol acetate, butyl cellosolve acetate, propene carbonate,
In DMSO, dimethyl succinate, propylene glycol methyl ether acetate, NMP, dimethylbenzene, dibutyl phthalate, dimethyl carbonate
One or more kinds of in the mixed solvents.Then graphite is added in the solution, 30-60min is soaked at 40-60 DEG C,
To complete special adsorption of the surfactant to graphite edge.
Step S2, a mechanical shear stress, the intensity size of the mechanical shear stress are applied to the graphite after immersion-organic solution
For 3000-7000psi, the time for applying shearing force is 1-5h, wherein the mode for imposing mechanical shear stress can be Supersonic
Ripple concussion (ultrasonication), mixed at high speed (high speed mixing), normal pressure uniformly mix (homogenizer),
Planetary bead mill (planet bead milling), high-pressure fluid uniformly mix (high pressure homogenizer) extremely
It is one of few.
Step S3, is filtered to the graphene suspension after mechanical stripping with the copper mesh of different meshes, obtains different chis
Very little distribution graphene suspension.
Step S4, weighs 40-100g conductive fillers respectively, and 10-30g binding agents, 0-20g auxiliary packings, 0-10g functions add
Plus agent, the highly conductive polymeric dispersants of 0-5g.Then binding agent is added in graphene suspension, be stirred at room temperature molten
Conductive filler, auxiliary packing, functional additive, highly conductive polymeric dispersant, are then added in the solution, in vacuum by solution
In stir, produce graphene conductive slurry.
Preferably, conductive filler is selected from copper powder, silver powder, aluminium powder or aluminium alloy, nickel powder, CNT, conductive carbon fibre, second
Any of acetylene black, conductive titanium dioxide, conductive ferrorphosphorus powder or two or more combinations.
Preferably, binding agent, which is selected from, includes phenolic resin, epoxy resin, polyester resin, vinylite, polyurethane tree
Any of fat, polyketone resin, ethyl cellulose or two or more combinations.
Preferably, auxiliary packing includes any in glass dust, SnO2, ZnO, Al2O3, TiO2, SiO2
One or two kinds of combination of the above.
Preferably, selection VTES as coupling agent, BYK-161 as advection agent,
Ethanol is as defoamer and sagging inhibitor, and sodium carboxymethylcellulose is dispersant.
Embodiment 1
（1）Under 60 DEG C of magnetic agitation effects, by 10g tetrabutyls ammonium bicarbonate solubility in 190g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 3000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 30min.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 2
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 3000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 30min.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 3
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 0min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 3000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 30min.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 4
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 3000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 30min.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 5
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 5000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 30min.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 6
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is using mechanical attrition method to stone
Ink applies the mechanical shear stress that intensity size is 5000psi, and machinery is carried out to intercalated graphite in the presence of this mechanical shear stress
Peel off, the mechanical stripping time is 1h.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Embodiment 7
（1）Under 60 DEG C of magnetic agitation effects, by 30g tetrabutyls ammonium bicarbonate solubility in 170g propylene carbonate solvents
In, prepare the carbonic allyl ester solution with surfactant.
（2）Particle diameter is immersed in step for 300 μm of graphite（1）In obtained carbonic allyl ester solution, lived on surface
The intercalation to graphite particle edge is completed in the presence of property agent, soak time is 30min.
（3）By step（2）Middle graphite-organic solution after surfactant intercalated processing is shelled using ultrasonic method
From, ultrasonic power be the 500W mechanical stripping times be 1h.
（4）By step（3）The middle graphene suspension after mechanical stripping carries out filtration treatment using the copper mesh of 300 mesh,
Obtain the more uniform graphene suspension of graphene particles size distribution.
（5）Measure 100g steps（4）In the graphene suspension that is filtrated to get, 10g ethyl celluloses are led at room temperature
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by 50g 10nm silver powder, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agents, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethylcelluloses be added to dissolved with
In the graphene suspension of binding agent, 3h is stirred in a vacuum, obtains graphene conductive slurry.
Claims (6)
1. a kind of method that mechanical stripping prepares graphene conductive slurry, it is characterised in that comprise the following steps：
Step S1, at 50-80 DEG C, by the 10-40g tetramethyl ammonium hydrogen carbonates weighed, tetraethyl ammonium hydrogen carbonate, tetrabutyl carbonic acid
A kind of surfactant in hydrogen ammonium is dissolved in 160-190g butyl acetates, diethyl carbonate, DBE, ethyl under magnetic stirring
Carbitol acetate, methyl ethyl carbonate, butyl carbitol acetate, butyl cellosolve acetate, propene carbonate, DMSO, fourth
One kind in acid dimethyl, propylene glycol methyl ether acetate, NMP, dimethylbenzene, dibutyl phthalate, dimethyl carbonate or
Graphite, is then added in the solution by two or more in the mixed solvents, and 30-60min is soaked at 40-60 DEG C, completes table
Special adsorption of the face activating agent to graphite edge；
Step S2, a mechanical shear stress is applied to the graphite after immersion-organic solution, and the intensity size of the mechanical shear stress is
3000-7000psi, wherein impose the mode of mechanical shear stress uniformly mixed for ultrasonic vibrating, mixed at high speed, normal pressure, planet
Formula bead mill, high-pressure fluid uniformly mix at least one；
Step S3, is filtered to the graphene suspension after mechanical stripping with the copper mesh of 300 mesh, obtains graphene suspension；
Step S4, weighs 40-100g conductive fillers, 10-30g binding agents, 0-20g auxiliary packings, the addition of 0-10g functions respectively
Binding agent, is then added in graphene suspension by agent, the highly conductive polymeric dispersants of 0-5g, and dissolving is stirred at room temperature,
Then conductive filler, auxiliary packing, functional additive, highly conductive polymeric dispersant are added in the solution, in a vacuum
Stir, produce graphene conductive slurry.
2. the method that mechanical stripping prepares graphene conductive slurry according to claim 1, it is characterised in that highly conductive polymerization
Thing dispersant includes being sodium carboxymethylcellulose, Sodium Polyacrylate, POLYPROPYLENE GLYCOL, neopelex, fatty acid glycerine
Combination more than one or both of ester, triethanolamine soap.
3. the method that mechanical stripping prepares graphene conductive slurry according to claim 1, it is characterised in that the conduction is filled out
Material is selected from copper powder, silver powder, aluminium powder, aluminium alloy, nickel powder, CNT, conductive carbon fibre, acetylene black, conductive titanium dioxide, conductive phosphorus
Any of iron alloy powder or two or more combinations.
4. the method that mechanical stripping prepares graphene conductive slurry according to claim 1, it is characterised in that the binding agent
For appointing in phenolic resin, epoxy resin, polyester resin, vinylite, polyurethane resin, polyketone resin, ethyl cellulose
One or more kinds of combinations.
5. the method that mechanical stripping prepares graphene conductive slurry according to claim 1, it is characterised in that the auxiliary is filled out
Expect for glass dust, SnO2、ZnO、Al2O3、TiO2、SiO2Any one of or two or more combinations.
6. the method that mechanical stripping prepares graphene conductive slurry according to claim 1, it is characterised in that binding agent is molten
Conductive filler, auxiliary packing, functional additive, highly conductive polymeric dispersant are added and suspended in after graphene suspension by solution
In liquid, then mechanical agitation is uniform.
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| CN114306753B (en) * | 2021-12-15 | 2023-02-24 | 海宁市产业技术研究院 | Implantable electric stimulation conductive stent and preparation method thereof |
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| CN103373724A (en) * | 2012-04-17 | 2013-10-30 | 安炬科技股份有限公司 | Method for preparing graphene composite material |
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