CN105869770A - Graphene conductive paste prepared by mechanical stripping and preparation method of graphene conductive paste - Google Patents
Graphene conductive paste prepared by mechanical stripping and preparation method of graphene conductive paste Download PDFInfo
- Publication number
- CN105869770A CN105869770A CN201610189835.5A CN201610189835A CN105869770A CN 105869770 A CN105869770 A CN 105869770A CN 201610189835 A CN201610189835 A CN 201610189835A CN 105869770 A CN105869770 A CN 105869770A
- Authority
- CN
- China
- Prior art keywords
- graphene
- mechanical stripping
- graphene conductive
- slurry
- suspension
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
The invention discloses a graphene conductive paste prepared by mechanical stripping and a preparation method of the graphene conductive paste. The paste is prepared from the following components by percentage: 50%-80% of graphene suspension, 20%-50% of a conductive filler, 5%-15% of a binder, 0-10% of an auxiliary filler, 0-5% of a functional additive and 0-5% of a high conductive polymer dispersant. The preparation method comprises the following steps: firstly, carrying out intercalation treatment on graphene in an organic solvent by a high molecular surfactant; secondly, preparing the graphene suspension through mechanical stripping and then carrying out filtering treatment on the mechanically stripped suspension; and finally, adding the conductive filler, the binder, the auxiliary filler and the functional additive for stirring evenly to obtain the graphene conductive paste. Intercalation treatment is carried out by the surfactant to protect the structural integrity of the graphene; the graphene conductive paste is directly prepared by a one-step method; the complicated technological process of firstly preparing the graphene and then preparing the conductive paste is simplified; and the electrical property of the graphene conductive paste and the dispersity and the stability of the paste are also improved.
Description
Technical field
The method that the present invention relates to use mechanical stripping to prepare graphene conductive slurry in organic solvent.
Background technology
2004, Univ Manchester UK peace moral strong K Hai Mu professor and Constantine. Nuo Woxiao love professor
First passage adhesive tape stripping means is prepared for single-layer graphene, and Graphene becomes the research heat of material supply section educational circles of the world subsequently
Point.By constantly finding its research, Graphene has mechanics, calorifics, electric property and the optical property of excellence, under room temperature its
Electron mobility is up to 15000 cm2/V s, and the movement velocity of electronics has reached the 1/300 of the light velocity, and resistivity only about 10-6
Ω cm is lower than copper or silver.Compared with conventional conductive slurry, graphene conductive slurry has more preferable electric property, extensively
It is applied to the fields such as microelectronic component, solaode, chemical cell, LED.
At present, the method preparing Graphene mainly has Physical and chemical method.Physical is mainly by the thing of storeroom
The Graphene with intrinsic property is prepared in reason effect, and it is the most completely chemical constitution that Graphene prepared by the method has, material
Material performance will not be destroyed, but the Graphene quality prepared is unstable, including mechanical stripping method, arc discharge method, ultrasonic method etc..
The most logical chemical reaction of chemical method prepares Graphene, and Graphene quality prepared by this method is relatively stable, but chemical reaction process
The intrinsic structure of middle Graphene may be destroyed, and causes the performance of Graphene to reduce.As used oxidation-reduction method to prepare graphite
In alkene materials process, oxy radical destroys the sp2 hybrid orbital in Graphene, defines sp3 hybrid orbital, greatly reduces
The electric conductivity of Graphene.Chemical method mainly has organic synthesis method, chemical vapour deposition technique, oxidation-reduction method etc..Pass through
Research for a long time, the method preparing Graphene gets more and more, and technology is also gradually improved, it is achieved that large-scale production, but
But report is rarely had about Graphene application in electrocondution slurry.
Invent herein and first high molecular surfactant is carried out intercalation processing to graphite, use the most in organic solvent
Graphite after processing is peeled off by the method for mechanical stripping, is then processed by suspension, directly prepares graphene conductive
Slurry.Although about preparing the patent of graphene conductive slurry it has been reported that but use one-step method to prepare graphene conductive slurry
The patent of material is not yet reported.Patent 201510239652.5 reports employing inorganic strong oxidizer and graphite is carried out intercalation processing,
Then it is prepared for Graphene by ultrasonic method.The method uses strong oxidizer to process the chemical constitution being easily destroyed graphite, makes
Sp2 hybrid orbital reduces, and causes the hydraulic performance decline of Graphene, and the present invention uses organic polymer to carry out graphite at intercalation
Reason, is conducive to protecting the chemical constitution of Graphene.Patent 201510713784.7 uses high molecular surfactant to enter graphite
Row intercalation processing, is then by mechanically pulling off and is prepared for Graphene, and by regulating the hydrophilic parent of high molecular surfactant
Oil equilibrium valve (HLB) is to regulate the compatibility between surfactant and different solvents, thus improves mechanical stripping efficiency.But should
Scheme mainly studies the preparation of surfactant, does not study graphene conductive slurry.Patent 201410828734.9
Propose use inorganic dispersant and graphenic surface is carried out adsorption treatment, to improve Graphene easily sending out in electrocondution slurry
The raw problem reunited.Although using inorganic dispersant that Graphene carries out process can reduce the reunion between Graphene, but
Still cannot solve its uniformity and stability problem.The present invention uses high molecular surfactant to prepare Graphene, directly obtains
Must have the suspension of preferable dispersive property, the most directly carry out the preparation of electrocondution slurry, simplify and make after first preparing Graphene
Standby graphene conductive slurry technical process.And later stage addition high connductivity polymer improves dividing of graphene conductive slurry further
Dissipate property and stability.
Summary of the invention
A kind of mechanical stripping of offer is provided and prepares graphene conductive slurry and preparation method thereof, should
Method mainly includes that three processes prepared by the intercalation processing of graphite, the preparation of graphene suspension, graphene conductive slurry.Use
High molecular surfactant carries out intercalation processing to graphite, to improve mechanical stripping efficiency, and protects Graphene result at machinery
It is not destroyed during stripping.Then filler, functional additive etc. are added in the suspension after copper mesh filters and prepare stone
Ink alkene electrocondution slurry.The present invention protects the graphene conductive slurry being prepared gained by preparation method of the present invention further.
Preparing graphene conductive slurry for realizing above-mentioned one-step method, this technical scheme comprises the steps:
After A carries out intercalation processing by high molecular surfactant to graphite, through mechanical stripping and filter process preparation
The more uniform graphene suspension of grain size.
B mechanical stripping prepares the percentage composition of graphene conductive slurry: graphene suspension 50-80%, conduction
Filler 20-50%, binding agent 5-15%, auxiliary packing 0-10%, functional additive 0-5%, high connductivity polymeric dispersant 0-5%.
According to step A, will be selected from tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate, dodecyl
In at least one surfactant solution organic solvent in tetramethyl guanidine carbonate and cetyl tetramethylammonium guanidine carbonate.
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, Allyl carbonate, DMSO, dimethyl succinate, propylene glycol monomethyl ether
Any one or more in acetate, NMP, dimethylbenzene, dibutyl phthalate, dimethyl carbonate and diphenyl carbonate
Combination.
According to step A, graphite is joined dissolved with in the organic solution of surfactant.
Preferably, graphite soaks 30-60min in organic solution, in order to be sufficiently complete intercalation process.
According to step A, use ball milling, Ball-stirring mill method, ultrasonic at least one graphite-organic solution mixture is carried out
Mechanical stripping.
According to step A, the graphite-organic solution after mechanical stripping is carried out filtration treatment through the copper mesh of 300 mesh, takes filtration
After suspension standby.
According to step B, it is preferred that Graphene is homemade graphene suspension in step A.
According to step B, further, conductive filler selected from copper powder, argentum powder, aluminium powder or aluminium alloy, nikel powder, CNT,
Conductive carbon fibre, acetylene black, conductive titanium dioxide, conduction ferrorphosphorus powder, in the combination of any one or more.
According to step B, further, binding agent is selected from including phenolic resin, epoxy resin, polyester resin, vinyl tree
The combination of any one or more in fat, polyurethane resin, polyketone resin, ethyl cellulose.
According to step B, further, appointing during auxiliary packing includes glass dust, SnO2, ZnO, Al2O3, TiO2, SiO2
What one or two kinds of combination of the above.
According to step B, further, selecting VTES as coupling agent, BYK-161 is as advection
Agent, ethanol is as defoamer and sagging inhibitor.
According to step B, further, selection sodium carboxymethyl cellulose is dispersant, to improve slurry dispersibility and to stablize
Property.
According to step B, the preparation process of graphene conductive slurry is as follows:
Mass percent according to graphene conductive slurry weighs graphene suspension and the organic binder bond of certain mass,
At 60-80 DEG C, by stirring by binder solution graphene suspension.
The conductive filler of certain mass, auxiliary packing, functional additive, dispersant is weighed according to slurry percentage composition,
It is stirred mixing with the graphene suspension being dissolved with adhesive by it.
As preferably, the stirring of slurry is vacuum stirring mix homogeneously at 30-60 DEG C, obtains graphene conductive slurry.
The present invention has an advantage compared with other methods preparing slurry:
The present invention, directly with graphite as raw material, uses one-step method directly to prepare graphene conductive slurry.It is graphite with reporting
Alkene electrocondution slurry preparation method is compared, and the method eliminates first prepares Graphene, then the Graphene obtained is prepared as conductive paste
The tedious steps of material.
Preparing graphene suspension during the course, carrying out intercalation with high molecular surfactant, it is to avoid use strong oxygen
Agent carries out intercalation and destroys the problem of intrinsic Graphene chemical constitution, is conducive to protecting graphene-structured, improves the conduction of slurry
Performance.
The present invention uses high connductivity polymers carboxymethylcellulo,e sodium to make as the dispersant of slurry, the patent more reported
As dispersant, there is more preferable dispersion effect with inorganic carbon dust, can preferably improve the uniformly dispersed of graphene conductive slurry
And stability.
Accompanying drawing explanation
Fig. 1 is the process chart that in the present invention, mechanical stripping prepares conductive graphene.
Specific embodiments
Understand the technology of the present invention for convenience, illustrate below in conjunction with the accompanying drawings technical scheme is described in detail.The present invention with
Graphite is raw material, and uses after in organic solvent graphite being carried out intercalation processing mechanical stripping method to prepare graphene suspension,
Graphene conductive slurry is prepared on this basis, to improve the electric conductivity of slurry, to divide by interpolation high connductivity polymeric dispersant
Dissipate property and stability.According to accompanying drawing 1, this technical scheme mainly includes four steps, and the intercalation processing of S1 graphite, at S2 intercalation
The mechanical stripping of the graphite after reason, after S3 mechanical stripping, graphene suspension is prepared in filtration, and S4 is prepared by graphene suspension
Electrocondution slurry.
Step S1, at 50-80 DEG C, by the 10-40g tetramethyl ammonium hydrogen carbonate weighed, tetraethyl ammonium hydrogen carbonate, the tetrabutyl
A kind of surfactant in ammonium hydrogen carbonate be dissolved under magnetic stirring 160-190g butyl acetate, diethyl carbonate, DBE,
Ethyl carbitol acetate, Ethyl methyl carbonate, butyl carbitol acetate, butyl cellosolve acetate, Allyl carbonate,
In DMSO, dimethyl succinate, propylene glycol methyl ether acetate, NMP, dimethylbenzene, dibutyl phthalate, dimethyl carbonate
In one or more mixed solvent.Then graphite is joined in this solution, at 40-60 DEG C, soaks 30-60min,
To complete the surfactant special adsorption to graphite edge.
Step S2, applies a mechanical shear stress to the graphite-organic solution after soaking, the intensity size of this mechanical shear stress
For 3000-7000psi, the time applying shear action is 1-5h, and the mode wherein imposing mechanical shear stress can be Supersonic
Ripple concussion (ultrasonication), mixed at high speed (high speed mixing), normal pressure uniformly mixed (homogenizer),
Planetary bead mill (planet bead milling), high-pressure fluid uniformly mix (high pressure homogenizer) extremely
Lack one of them.
Step S3, filters the graphene suspension after mechanical stripping with the copper mesh of different meshes, obtains different chi
Very little distribution graphene suspension.
Step S4, weighs 40-100g conductive filler, 10-30g binding agent, 0-20g auxiliary packing respectively, and 0-10g function adds
Add agent, 0-5g high connductivity polymeric dispersant.Then binding agent is joined in graphene suspension, be stirred at room temperature molten
Solve, then conductive filler, auxiliary packing, functional additive, high connductivity polymeric dispersant are joined in this solution, in vacuum
In stir, obtain graphene conductive slurry.
Preferably, conductive filler is selected from copper powder, argentum powder, aluminium powder or aluminium alloy, nikel powder, CNT, conductive carbon fibre, second
The combination of any one or more in acetylene black, conductive titanium dioxide, conduction ferrorphosphorus powder.
Preferably, binding agent is selected from including phenolic resin, epoxy resin, polyester resin, vinylite, polyurethane tree
The combination of any one or more in fat, polyketone resin, ethyl cellulose.
Preferably, any during auxiliary packing includes glass dust, SnO2, ZnO, Al2O3, TiO2, SiO2
One or two kinds of combination of the above.
Preferably, select VTES as coupling agent, BYK-161 as advection agent,
Ethanol is as defoamer and sagging inhibitor, and sodium carboxymethyl cellulose is dispersant.
Embodiment 1
(1) under 60 DEG C of magnetic agitation effects, by 10g tetrabutyl ammonium bicarbonate solubility in 190g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 3000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 30min.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 2
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 3000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 30min.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 3
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 0min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 3000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 30min.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 4
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 3000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 30min.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 5
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 5000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 30min.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 6
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) use mechanical attrition method to stone graphite after surfactant intercalated process in step (2)-organic solution
It is the mechanical shear stress of 5000psi that ink applies intensity size, under the effect of this mechanical shear stress, intercalated graphite is carried out machinery
Peeling off, the mechanical stripping time is 1h.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Embodiment 7
(1) under 60 DEG C of magnetic agitation effects, by 30g tetrabutyl ammonium bicarbonate solubility in 170g propylene carbonate solvent, system
Get everything ready the carbonic allyl ester solution of surfactant.
(2) graphite that particle diameter is 300 μm is immersed in the carbonic allyl ester solution obtained by step (1), lives on surface
Completing the intercalation to graphite granule edge under the effect of property agent, soak time is 30min.
(3) ultrasonic method is used to shell graphite after surfactant intercalated process in step (2)-organic solution
From, ultrasonic power be the 500W mechanical stripping time be 1h.
(4) copper mesh of 300 mesh is used to carry out filtration treatment graphene suspension after mechanical stripping in step (3),
Obtain the more uniform graphene suspension of Graphene particle size distribution.
(5) measure the graphene suspension being filtrated to get in 100g step (4), 10g ethyl cellulose is at room temperature led to
Crossing magnetic agitation effect, to be dissolved in graphene suspension total.Then by the argentum powder of 50g 10nm, 20g glass dust, 2g vinyl three
Ethoxysilane, 1g BYK-161 advection agent, 1g ethanol, 2g sagging inhibitor and 4g sodium carboxymethyl cellulose join dissolved with
In the graphene suspension of binding agent, stir 3h in a vacuum, obtain graphene conductive slurry.
Claims (10)
1. the method that a mechanical stripping prepares graphene conductive slurry, it is characterised in that comprise the steps:
Being joined by high molecular surfactant in organic solvent, preparation has the solution of surfactant, is poured into by graphite
Soak a period of time dissolved with in the solution of surfactant；Then graphite and the solution through surfactant intercalated process is used
The method of mechanical stripping prepares Graphene slurry；The copper mesh that slurry after mechanical stripping uses 300 mesh carries out filtration treatment, takes
Suspension after filtration prepares graphene conductive slurry；Add high conducting polymer when preparing electrocondution slurry and lead to improve Graphene
The dispersibility of plasma-based material and stability.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that live in described surface
In property agent solution, the mass percent of surfactant is 5-20%.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that surfactant
Selected from tetramethyl ammonium hydrogen carbonate, tetraethyl ammonium hydrogen carbonate, tetrabutyl ammonium hydrogen carbonate, dodecyl tetramethyl guanidine carbonate and hexadecane
At least one in base tetramethyl guanidine carbonate.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that second chosen by solvent
Acid butyl ester, diethyl carbonate, DBE, ethyl carbitol acetate, Ethyl methyl carbonate, butyl carbitol acetate, butyl cellosolve
Acetate, Allyl carbonate, DMSO, dimethyl succinate, propylene glycol methyl ether acetate, NMP, dimethylbenzene, phthalic acid two
The combination of any one or more in butyl ester, dimethyl carbonate and diphenyl carbonate.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that mechanical stripping selects
By ball-milling method, ultrasonic, Ball-stirring mill method.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that by mechanical stripping
After solution filter with the copper mesh of 300 mesh, in order to obtain the graphene suspension of even particle size.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that electrocondution slurry
Composition: graphene suspension 50-80%, conductive filler 20-50%, binding agent 5-15%, auxiliary packing 0-10%, functional additive
0-5%, high connductivity polymeric dispersant 1-5%.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that high connductivity is polymerized
Thing dispersant include sodium carboxymethyl cellulose, sodium polyacrylate, POLYPROPYLENE GLYCOL, dodecylbenzene sodium sulfonate, fatty glyceride,
One or more combination in triethanolamine soap.
The method that the most according to claim 1, mechanical stripping prepares graphene conductive slurry, it is characterised in that binding agent is molten
Conductive filler, auxiliary packing, functional additive, high connductivity polymer, after graphene suspension, are added in suspension, so by solution
Rear mechanical agitation is uniform.
10. a graphene conductive slurry, it is characterised in that prepared the graphite of gained by claim 1-9 any one preparation method
Alkene electrocondution slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610189835.5A CN105869770B (en) | 2016-03-30 | 2016-03-30 | A kind of mechanical stripping prepares graphene conductive slurry and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610189835.5A CN105869770B (en) | 2016-03-30 | 2016-03-30 | A kind of mechanical stripping prepares graphene conductive slurry and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105869770A true CN105869770A (en) | 2016-08-17 |
| CN105869770B CN105869770B (en) | 2017-10-27 |
Family
ID=56627409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610189835.5A Active CN105869770B (en) | 2016-03-30 | 2016-03-30 | A kind of mechanical stripping prepares graphene conductive slurry and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105869770B (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328240A (en) * | 2016-08-20 | 2017-01-11 | 张伟 | Organic polymer-based composite graphene electrode material and preparation method therefor |
| CN106564888A (en) * | 2016-10-26 | 2017-04-19 | 成都新柯力化工科技有限公司 | Method of preparing graphene nanoplate size through nanometer-distribution collision stripping and graphene nanoplate size |
| CN106566302A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene composite dispersion liquid for anticorrosion coating and preparation method thereof |
| CN106589903A (en) * | 2016-12-09 | 2017-04-26 | 四川大学 | Preparation method and application of graphene polyurethane nanocomposite |
| CN107265445A (en) * | 2017-07-06 | 2017-10-20 | 东南大学 | A kind of green high-efficient of high-quality graphene prepares method |
| CN108305702A (en) * | 2018-01-19 | 2018-07-20 | 林荣铨 | A kind of preparation and its application of medium temperature graphene/silver composite conducting slurry |
| CN108305703A (en) * | 2018-01-19 | 2018-07-20 | 林荣铨 | A kind of preparation and its application of medium temperature graphene/nickel composite conducting slurry |
| CN108529606A (en) * | 2017-03-03 | 2018-09-14 | 江苏天奈科技股份有限公司 | A kind of graphene slurry of high stability and preparation method thereof |
| CN108630338A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom |
| CN110304621A (en) * | 2018-03-20 | 2019-10-08 | 国家纳米科学中心 | For by the slurry of predetermined pattern redox graphene, application method and obtained graphene film layer |
| CN110983759A (en) * | 2019-12-19 | 2020-04-10 | 青岛墨金烯碳新材料科技有限公司 | Graphene modified carbon fiber pre-vulcanized fiber fabric and preparation method thereof |
| CN113698802A (en) * | 2021-08-24 | 2021-11-26 | 成都新柯力化工科技有限公司 | Graphene hybridized organic-inorganic anticorrosive paint and preparation method thereof |
| CN114068065A (en) * | 2021-03-10 | 2022-02-18 | 杭州安誉科技有限公司 | Conductive material for temperature sensor and use thereof |
| CN114306753A (en) * | 2021-12-15 | 2022-04-12 | 海宁市产业技术研究院 | Implantable electric stimulation conductive stent and preparation method thereof |
| CN116798699A (en) * | 2023-08-29 | 2023-09-22 | 苏州迪天机器人自动化有限公司 | Process for manufacturing conductive paste and intermediate skin layer for touch sensor |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN103373724A (en) * | 2012-04-17 | 2013-10-30 | 安炬科技股份有限公司 | Method for preparing graphene composite material |
| KR20130128804A (en) * | 2012-05-18 | 2013-11-27 | 채규종 | Toddler chair |
| CN104261394A (en) * | 2014-09-25 | 2015-01-07 | 深圳粤网节能技术服务有限公司 | Preparation method of graphene |
| CN104464883A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Graphene electrocondution slurry with dispersants adsorbed on surface and manufacturing method and application thereof |
| CN104966837A (en) * | 2015-04-24 | 2015-10-07 | 深圳市德方纳米科技股份有限公司 | Graphene conductive liquid as well as preparation method and application thereof |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
-
2016
- 2016-03-30 CN CN201610189835.5A patent/CN105869770B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN103373724A (en) * | 2012-04-17 | 2013-10-30 | 安炬科技股份有限公司 | Method for preparing graphene composite material |
| KR20130128804A (en) * | 2012-05-18 | 2013-11-27 | 채규종 | Toddler chair |
| CN104261394A (en) * | 2014-09-25 | 2015-01-07 | 深圳粤网节能技术服务有限公司 | Preparation method of graphene |
| CN104464883A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Graphene electrocondution slurry with dispersants adsorbed on surface and manufacturing method and application thereof |
| CN104966837A (en) * | 2015-04-24 | 2015-10-07 | 深圳市德方纳米科技股份有限公司 | Graphene conductive liquid as well as preparation method and application thereof |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328240A (en) * | 2016-08-20 | 2017-01-11 | 张伟 | Organic polymer-based composite graphene electrode material and preparation method therefor |
| CN109087724B (en) * | 2016-08-20 | 2020-08-14 | 山西省太谷县宝光碳素有限公司 | Preparation method of graphene electrode material |
| CN109087724A (en) * | 2016-08-20 | 2018-12-25 | 漳州龙文区信创友工业设计有限公司 | A kind of preparation method of Graphene electrodes material |
| CN106566302B (en) * | 2016-10-20 | 2018-05-11 | 深圳市蓝水海洋高端装备研究院有限公司 | A kind of graphene composite dispersion liquid for anticorrosive paint and preparation method thereof |
| CN106566302A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene composite dispersion liquid for anticorrosion coating and preparation method thereof |
| CN106564888A (en) * | 2016-10-26 | 2017-04-19 | 成都新柯力化工科技有限公司 | Method of preparing graphene nanoplate size through nanometer-distribution collision stripping and graphene nanoplate size |
| CN106589903A (en) * | 2016-12-09 | 2017-04-26 | 四川大学 | Preparation method and application of graphene polyurethane nanocomposite |
| CN108529606A (en) * | 2017-03-03 | 2018-09-14 | 江苏天奈科技股份有限公司 | A kind of graphene slurry of high stability and preparation method thereof |
| CN107265445A (en) * | 2017-07-06 | 2017-10-20 | 东南大学 | A kind of green high-efficient of high-quality graphene prepares method |
| CN108305702A (en) * | 2018-01-19 | 2018-07-20 | 林荣铨 | A kind of preparation and its application of medium temperature graphene/silver composite conducting slurry |
| CN108305703A (en) * | 2018-01-19 | 2018-07-20 | 林荣铨 | A kind of preparation and its application of medium temperature graphene/nickel composite conducting slurry |
| CN108630338A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom |
| CN110304621A (en) * | 2018-03-20 | 2019-10-08 | 国家纳米科学中心 | For by the slurry of predetermined pattern redox graphene, application method and obtained graphene film layer |
| CN110983759A (en) * | 2019-12-19 | 2020-04-10 | 青岛墨金烯碳新材料科技有限公司 | Graphene modified carbon fiber pre-vulcanized fiber fabric and preparation method thereof |
| CN114068065A (en) * | 2021-03-10 | 2022-02-18 | 杭州安誉科技有限公司 | Conductive material for temperature sensor and use thereof |
| CN113698802A (en) * | 2021-08-24 | 2021-11-26 | 成都新柯力化工科技有限公司 | Graphene hybridized organic-inorganic anticorrosive paint and preparation method thereof |
| CN113698802B (en) * | 2021-08-24 | 2022-04-22 | 金隅微观（沧州）化工有限公司 | Graphene hybridized organic-inorganic anticorrosive paint and preparation method thereof |
| CN114306753A (en) * | 2021-12-15 | 2022-04-12 | 海宁市产业技术研究院 | Implantable electric stimulation conductive stent and preparation method thereof |
| 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 |
| CN116798699A (en) * | 2023-08-29 | 2023-09-22 | 苏州迪天机器人自动化有限公司 | Process for manufacturing conductive paste and intermediate skin layer for touch sensor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105869770B (en) | 2017-10-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105869770A (en) | Graphene conductive paste prepared by mechanical stripping and preparation method of graphene conductive paste | |
| CN105110318B (en) | A kind of graphene water paste and preparation method thereof | |
| CN104226980B (en) | The method strengthening metal powder material laser energy absorption efficiency | |
| CN1290121C (en) | Photosensitive silver slurry for concentration electrode and method for preparing same | |
| CN106185895A (en) | A kind of graphene dispersion liquid and preparation method thereof | |
| CN107674505A (en) | A kind of Graphene conductive ink and preparation method thereof | |
| CN108134090A (en) | A kind of nanometer of bismuth/carbon composite and preparation method thereof | |
| US20170117422A1 (en) | Silver paste for solar cell and method for making same | |
| CN106887270A (en) | A kind of depth-width ratio solar energy front side silver paste high and preparation method thereof | |
| CN104445169A (en) | Method for preparing grapheme by means of aqueous phase cutting and stripping | |
| CN105905888B (en) | A kind of compound microplate of graphene peeled off using turbine sand mill and preparation method thereof | |
| CN104772156A (en) | Preparation method for graphene loaded cobalt nickel phosphide composite material | |
| CN102360584B (en) | Carbon black additive-contained conductive slurry utilized by photovoltaic cell and preparation method thereof | |
| CN106543805B (en) | High-solid content polyvinyl chloride film gravure white ink and preparation method thereof | |
| CN102983306A (en) | Method for preparing negative pole slurry for lithium ion batteries | |
| CN102627272A (en) | Method for preparing less layer graphene sheet | |
| CN104103823B (en) | A kind of layering Li 4ti 5o 12the preparation method of graphene complex lithium ion battery cathode material | |
| CN104355308A (en) | Preparation method of graphene with large specific surface area | |
| CN106410210B (en) | A kind of preparation method of metal hydride/nano carbon composite material | |
| CN105590756B (en) | A kind of preparation method of micro/nano-scale graphene/lithium titanate composite anode material | |
| CN108134091A (en) | A kind of nanometer tin/carbon composite and preparation method thereof | |
| CN105140523A (en) | Flexible thin film electrode material for lithium ion battery and preparing method of flexible thin film electrode material | |
| CN106299356B (en) | A kind of lithium ion battery lithium vanadate Li3VO4The efficient microwave radiation synthesis process of nano flower | |
| CN111073396A (en) | Graphene-based water-based conductive ink and preparation method thereof | |
| CN107086297A (en) | A kind of preparation method of silicon-carbon cathode material and the silicon-carbon cathode material prepared using this method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210127 Address after: Room 808, 218 Ningguo Road, Yangpu District, Shanghai Patentee after: Xinhua (Shanghai) equipment Co., Ltd Address before: 610091, Sichuan, Chengdu province Qingyang dragon industrial port, East Sea 4 Patentee before: CHENGDU NEW KELI CHEMICAL SCIENCE Co.,Ltd. |