CN103319954B - Conductive graphene printing ink and preparation method thereof - Google Patents
Conductive graphene printing ink and preparation method thereof Download PDFInfo
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Abstract
The invention provides a conductive graphene printing ink. The conductive graphene printing ink is composed of 0.001-80wt% of graphene, 1-60wt% of a linking material, 0.1-30wt% of an assistant, and the balance solvent. The invention also provides a preparation method of the conductive graphene printing ink. The conductive graphene printing ink has the advantages of good toughness, good die molding performance, good adhesion and good impact resistance; chemically doped graphene and chemically modified graphene in the graphene have good conductive, mechanical and thermal performances. The molecules of the chemically doped graphene comprise one or more of polyaniline, polyacetylene, polythiophene, polyparaphenylene and polypyrrole, and the functional groups of the chemically modified graphene comprise one or more of an anilino group, a pyrryl group, an imidazolyl group, a benzenesulfonic acid group, a thienyl group, a furyl group, a phenyl group, a hydroxy group, an ester group and derivative groups thereof, so the conductive performance, the mechanical performances and the dispersion stability of graphene in the printing ink are improved.
Description
Technical field
The present invention relates to electronic material printing technology, be specifically related to a kind of graphene conductive ink and preparation method thereof.
Background technology
Graphene is the novel material by carbon atom individual layer sheet structure.Since the physicist An Deliehaimu of Univ Manchester UK in 2004 and Constantine Nuo Woxiaoluofu successfully isolate after Graphene, about the physics and chemistry performance of Graphene and its focus that has been applied to research.It is reported that the thickness of Graphene only has 0.34 nanometer, in Graphene, the conduction velocity of electronics is 8 × 10
5m/s; Electric conductivity 1250 ~ 7000s/m; The thermal property steady heat conductance of Graphene is 3080 ~ 5150W/mK.Graphene has superhard mechanical strength, reaches 110 ~ 130 GPa, and (2630m/ g) etc. to have the specific surface area of super large.The special construction of Graphene makes it have excellent performance, and Graphene is carried out effective efficiency processing by cheap cost, can be used as well the packing material of polymer composites.
Electrically conductive ink is a kind of functional ink, has certain electroconductibility and antistatic effect, is widely used in printing PCB, unicircuit, the materials such as RF tag.The ink that traditional electrically conductive ink is all made up of gold and silver, copper powder or other metal powders or carbon dust and binder etc., cost is high, the shortcomings such as complex process, resistivity are high, forming and hardening temperature height, along with electronic product and equipment are to future developments such as light, thin, little, low cost, multi-functional, high reliability, the consumption of flexible circuit is increasing, utilize electrically conductive ink or conductive ink by the mode of printing or printing, on flexible insulation substrate, form conducting wire and attract wide attention.Graphene, as the emerging gang of carbon material, has good mechanical property and special Electronic Performance, makes the performance of Graphene/high polymer composite material more superior.Compared with existing nano metal (as nano-silver powder, copper nanoparticle etc.) electrically conductive ink, Graphene ink has huge cost advantage.Graphene can, by the passage of transfer transport is provided, make composite material conductive.
Graphene ink is the ink product with specific functions such as conductions of the compositions such as a class Graphene, binder, auxiliary agent and solvent, there is conductivity excellence, printed patterns quality is light, printability good, condition of cure is gentle and the advantage such as with low cost, can on the multiple base materials such as plastics film, paper and tinsel, realize printing.Graphene ink is applicable to the modes such as wire mark, gravure, flexo, offset printing and ink jet printing, the aspects such as printed-wiring board (PWB) (PCB), RF identification (RFID), display equipment (as OLED), electrode sensor can be applied to, organic solar batteries, printed battery can be potential be applied to and above ultracapacitor.Therefore Graphene ink is expected to be used widely in, flexible electronic product frivolous electronic radio frequency identification label, intelligent packaging, thin film switch, flexible circuit board and the sensor next generation, and market outlook are wide.
In sum, be necessary to carry out developing energetically in Graphene ink research field, a kind of Graphene ink finished product and preparation method thereof is provided.
summary of the invention
The object of the invention is to be achieved through the following technical solutions:
A kind of graphene conductive ink, it is made up of following compositions in weight percentage:
Graphene 0.001 wt% ~ 80 wt%; Low-melting ink vehicle 1 wt% ~ 60 wt%; Auxiliary agent 0.1 wt% ~ 30 wt%; Surplus is organic solvent.
As optimization, the lamellar spacing of described Graphene is that 0.34 nm ~ 100 nm, planar dimension are 0.001 μ m ~ 30 μ m; Described Graphene comprises the Graphene of do not adulterate unmodified Graphene and chemical doping, chemical modification, wherein the molecule of chemical doping Graphene comprises one or several between polyaniline, polyacetylene, Polythiophene, polyparaphenylene and polypyrrole, and there are one or several between anilino, pyrryl, imidazolyl, Phenylsulfonic acid base, thienyl, furyl, phenyl, hydroxyl, ester group and their deriveding group in the functional group of chemical modification Graphene.
As optimization, described low-melting ink vehicle comprises epoxy resin, Synolac, resol, aminoresin, vibrin, acrylic resin, urethane resin, chlorinated polyolefin resin, carbamide resin, silicone resin, fluorocarbon resin and the modified resin of various resins described in them, and one or more mixture in their centres.
As optimization, described epoxy resin is one or more the mixture in Racemic glycidol ethers bisphenol A-type, bisphenol f type epoxy resin, ethylene oxidic ester epoxy resin, aliphatic epoxy resin, cycloaliphatic epoxy resin, acrylic modified epoxy resin, polyurethane modified epoxy resin and modifying epoxy resin by organosilicon.
As optimization, described auxiliary agent comprise coupling agent, promotor, flow agent, defoamer, wetting dispersing agent and, in film coalescence aid and solidifying agent one or several etc.; Described coupling agent is silane coupling agent or titanate coupling agent; Described flow agent is acrylic acid or the like flow agent, fluorine class flow agent or organosilicon flow agent; Described promotor is Methylimidazole, 2-ethyl-4-methylimidazole or 3-aminopropyl imidazoles; Described defoamer is organo-siloxane, polyethers, silicon and ether grafting or amine; Described film coalescence aid is propandiol butyl ether, 1-Methoxy-2-propyl acetate or alcohol ester 12; Described solidifying agent is one or more the mixture in Dyhard RU 100, polymeric amide, diethylenetriamine, quadrol, diaminodiphenyl-methane, diaminodiphenylsulfone(DDS), Tetra hydro Phthalic anhydride, maleic anhydride and resol.
A preparation method for graphene conductive ink, to prepare its graphene conductive ink that contains 60 g bisphenol A epoxide resins as example, is characterized in that, it comprises the following steps:
Get 60 g bisphenol A epoxide resins and put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0 g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5 g defoamer solutions, 0.2 g promotor and 10 g vinyl acetic monomers while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 110 g Graphenes and mix with 150 g butanone, and add 1.1 g coupling agents to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500 r/ min and within 5 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
The preparation method of another kind of graphene conductive ink, to prepare its graphene conductive ink that contains 60 g bisphenol A epoxide resins as example, is characterized in that: it comprises the following steps:
Get 60 g bisphenol A epoxide resins and put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0 g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5 g defoamer solutions, 0.2 g promotor and 10 g vinyl acetic monomers while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 300 g Graphenes and mix with 400 g butanone, and add 3.0 g to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
The preparation method of another kind of graphene conductive ink, to prepare its graphene conductive ink that contains 60 g bisphenol A epoxide resins as example, is characterized in that: it comprises the following steps:
Get 60 g bisphenol A epoxide resins and put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0 g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5 g defoamer solutions, 0.2 g promotor and 10 g vinyl acetic monomers while stirring in described mixed solution, in homogenizer, disperse 2 hours, obtain binder;
Take 300 g Graphenes and mix with 400 g butanone, and add 3.0 g to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
The preparation method of another kind of graphene conductive ink, to prepare its graphene conductive ink that contains 60 g bisphenol A epoxide resins as example, is characterized in that: it comprises the following steps:
Get 60 g bisphenol A epoxide resins and put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0 g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5 g defoamer solutions, 0.2 g promotor and 10 g vinyl acetic monomers while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 300 g Graphenes and mix with 400 g butanone, and add 3.0 g to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
Compared with prior art, the present invention possesses following advantage:
Graphene comprises Graphene and chemical doping Graphene, chemical modification Graphene, and it has good conductivity, mechanical property, thermal property.The molecule of chemical doping Graphene comprises polyaniline, polyacetylene, Polythiophene, polyparaphenylene and polypyrrole, there are anilino, pyrryl, imidazolyl, Phenylsulfonic acid base, thienyl, furyl, phenyl, hydroxyl, ester group and their deriveding group in the functional group of chemical modification Graphene, and these groups can improve conductivity, the stably dispersing performance of Graphene in ink.
In described low-melting ink vehicle, epoxy resin contains epoxy group(ing), under solidifying agent effect and certain temperature condition, can form three-dimensional cross-linked curing compound, there is adhesiveproperties, the feature such as high shrinkage is little, cohesive force is strong, shrinking percentage is low, good stability, processing characteristics are good, be more that epoxy resin is carried out to modification, as acrylic modified epoxy resin, just have the features such as the gloss of acrylic resin, plentiful, good weatherability concurrently; Polyurethane modified epoxy resin, has good network structure, thereby improves epoxy resin toughness; Modifying epoxy resin by organosilicon can reduce epoxy resin internal stress, and the performance such as toughness, high thermal resistance that can improve again epoxy resin makes resin have good toughness, pressing mold performance, adhesiveproperties and erosion-resisting characteristics.Therefore, the ink taking epoxy resin as matrix has good sticking power, thermotolerance, snappiness etc.
Solidifying agent is and epoxy group(ing) generation open loop or the ring-closure reaction of epoxy resin, forms netted space polymer, and some matrix materials are coated among reticulate body.Be to carry out nucleophilic addition with epoxy resin as primary amine solidifies, each reactive hydrogen can be opened an epoxide group, makes it crosslinking curing.Hydroxyl and anhydride reaction on the epoxy resin of anhydride-cured chamber, generate ester bond and carboxylic acid, and carboxylic acid, again to epoxy group(ing) addition, generates hydroxyl, and the hydroxyl of generation continues to react this reaction process with other acid anhydride bases and repeatedly carries out, and generates three-dimensional polymer.
Graphene is monolithic layer structure, and electronics moves in aspect, conducts electricity very well like this, the coupling agent treatment that is epoxy group(ing) with end group, make more to mix with epoxy resin in graphene-structured, have the adhesion that has strengthened Graphene, thereby make ink there is good electroconductibility and sticking power.
Coupling agent in auxiliary agent contains inorganic group and organic group simultaneously, thereby the interface performance that improves resin and mineral filler improves the performance of matrix material greatly; Promotor can be shortened set time, reduces solidification value, reduces the effects such as hardener dose; Defoamer can be accelerated the speed of vacuum defoamation in glue, can also reduce sol solutions viscosity, improves application property, the dissolved glue film after solidifying, and smooth surface is without bubble etc.
embodiment
embodiment 1(comparative example)
Get 60 g bisphenol A epoxide resins (Hong Chang electronic material company, GESR901) put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100 (Gansu Daiei chemical industry, L-solidifying agent)-dimethyl formamide (BASF AG, A-801) the solution 11.0 g (ratio of Dyhard RU 100: dimethyl formamide=1:9, Dyhard RU 100 is fully dissolved in dimethyl formamide), in stirring, drip 1.5 g defoamer (Dow Corning Corporations, DC-56) solution, 0.2 g promotor (Gansu Daiei chemical industry, Methylimidazole) and 10 g vinyl acetic monomer (DOW Chemical, HCH), in homogenizer, disperse 1.5 hours, obtain binder,
By prepared binder by silk screen printing on PI film, thickness is about 10 microns, under certain condition solidify, with four point probe instrument test resistance rate be 1.2 × 10
-6Ω cm.
embodiment 2
Get 60 g bisphenol A epoxide resins (Hong Chang electronic material company, GESR901) put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100 (Gansu Daiei chemical industry, L-solidifying agent)-dimethyl formamide (BASF AG, A-801) the solution 11.0 g (ratio of Dyhard RU 100: dimethyl formamide=1:9, Dyhard RU 100 is fully dissolved in dimethyl formamide), in stirring, drip 1.5 g defoamer (Dow Corning Corporations, DC-56) solution, 0.2 g promotor (Gansu Daiei chemical industry, Methylimidazole) and 10 g vinyl acetic monomer (DOW Chemical, HCH), in homogenizer, disperse 1.5 hours, obtain binder,
Taking 110 g Graphenes (Ningbo Mo Xi Science and Technology Ltd.) mixes with 150 g butanone, and add 1.1 g coupling agent (DOW CORNINGs, Z-6040) put into ultrasonic apparatus and at 35 DEG C, carry out ultrasonic dispersion with 2500 r/ min and within 5 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In above-mentioned binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink;
By prepared graphene conductive ink by silk screen printing on PI film, thickness is about 10 microns, under certain condition solidify, with four point probe instrument test resistance rate be 6.1 × 10
-5Ω cm.
embodiment 3
Get 60 g bisphenol A epoxide resins (Hong Chang electronic material company, GESR901) put into test bottle, add 25 g butanone, stir 40 min until completely dissolved, add Dyhard RU 100 (Gansu Daiei chemical industry, L-solidifying agent)-dimethyl formamide (BASF AG, A-801) the solution 11.0 g (ratio of Dyhard RU 100: dimethyl formamide=1:9, Dyhard RU 100 is fully dissolved in dimethyl formamide), in stirring, drip 1.5 g defoamer (Dow Corning Corporations, DC-56) solution, 0.2 g promotor (Gansu Daiei chemical industry, Methylimidazole) and 10 g vinyl acetic monomer (DOW Chemical, HCH), in homogenizer, disperse 1.5 hours, obtain binder,
Taking 300 g Graphenes (Ningbo Mo Xi Science and Technology Ltd.) mixes with 400 g butanone, and add 3.0 g (DOW CORNINGs, Z-6040) put into ultrasonic apparatus and at 35 DEG C, carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In above-mentioned binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink;
By prepared graphene conductive ink by silk screen printing on PI film, thickness is about 10 microns, under certain condition solidify, with four point probe instrument test resistance rate be 4.3 × 10
-6Ω cm.
embodiment 4
(favour is contained chemical industry to get 60 g polyurethane modified epoxy resins, E-42) put into test bottle, add 25 g butanone, stir 45 min until completely dissolved, add 35 g maleic anhydride (Sartomers, SMA3000) and 0.8 g N, N-dimethyl benzylamine (A Faaisha company, A12191), in stirring, drip 1.5 g defoamers (Dow Corning Corporation, DC-56), 10 g vinyl acetic monomer (DOW Chemical, HCH), in homogenizer, disperse 2 hours, obtain binder stand-by;
Taking 300 g Graphenes (Ningbo Mo Xi Science and Technology Ltd.) mixes with 400 g butanone, and add 3.0 g (DOW CORNINGs, Z-6040) put into ultrasonic apparatus and at 35 DEG C, carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In above-mentioned binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink;
By prepared graphene conductive ink by silk screen printing on PI film, thickness is about 10 microns, under certain condition solidify, with four point probe instrument test resistance rate be 4.7 × 10
-6Ω cm.
embodiment 5
Get 60 g modifying epoxy resin by organosilicon (DOW CORNINGs, DC-0345) put into test bottle, add 25 g butanone, stir 45 min until diluting completely after dissolving, add 6 g polymeric amide, in stirring, drip 1.5 g defoamers (Dow Corning Corporation, DC-56), promotor (Gansu Daiei chemical industry, Methylimidazole) and 10 g vinyl acetic monomer (DOW Chemical, HCH), in homogenizer, disperse 1.5 hours, obtain binder;
Taking 300 g Graphenes (Ningbo Mo Xi Science and Technology Ltd.) mixes with 400 g butanone, and add 3.0 g (DOW CORNINGs, Z-6040) put into ultrasonic apparatus and at 35 DEG C, carry out ultrasonic dispersion with 2500 r/ min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In above-mentioned binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink;
By prepared graphene conductive ink by silk screen printing on PI film, thickness is about 10 microns, under certain condition solidify, with four point probe instrument test resistance rate be 4.6 × 10
-6Ω cm.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (5)
1. a graphene conductive ink, is characterized in that: it is made up of following compositions in weight percentage:
Graphene 0.001wt%～80wt%; Low-melting ink vehicle 1wt%～60wt%; Auxiliary agent 0.1wt%～30wt%; Surplus is organic solvent;
The lamellar spacing of described Graphene is that 0.34nm～100nm, planar dimension are 0.001 μ m～30 μ m; Described Graphene comprises the Graphene of do not adulterate unmodified Graphene and chemical doping, chemical modification, wherein the molecule of chemical doping Graphene comprises one or several between polyaniline, polyacetylene, Polythiophene, polyparaphenylene and polypyrrole, and there are one or several between anilino, pyrryl, imidazolyl, Phenylsulfonic acid base, thienyl, furyl, phenyl, hydroxyl, ester group and their deriveding group in the functional group of chemical modification Graphene;
Described low-melting ink vehicle comprises epoxy resin, Synolac, resol, aminoresin, vibrin, acrylic resin, urethane resin, chlorinated polyolefin resin, carbamide resin, silicone resin, fluorocarbon resin and the modified resin of various resins described in them, and one or more mixture in their centres;
Described epoxy resin is one or more the mixture in Racemic glycidol ethers bisphenol A-type, bisphenol f type epoxy resin, ethylene oxidic ester epoxy resin, aliphatic epoxy resin, cycloaliphatic epoxy resin, acrylic modified epoxy resin, polyurethane modified epoxy resin and modifying epoxy resin by organosilicon;
Described auxiliary agent comprises one or several in coupling agent, promotor, flow agent, defoamer, wetting dispersing agent, film coalescence aid and solidifying agent; Described coupling agent is silane coupling agent or titanate coupling agent; Described flow agent is acrylic acid or the like flow agent, fluorine class flow agent or organosilicon flow agent; Described promotor is Methylimidazole, 2-ethyl-4-methylimidazole or 3-aminopropyl imidazoles; Described defoamer is organo-siloxane or polyethers; Described film coalescence aid is propandiol butyl ether, 1-Methoxy-2-propyl acetate or alcohol ester 12; Described solidifying agent is one or more the mixture in Dyhard RU 100, polymeric amide, diethylenetriamine, quadrol, diaminodiphenyl-methane, diaminodiphenylsulfone(DDS), Tetra hydro Phthalic anhydride, maleic anhydride and resol.
2. a preparation method who contains the graphene conductive ink of 60g bisphenol A epoxide resin, is characterized in that, it comprises the following steps:
Get 60g bisphenol A epoxide resin and put into test bottle, add 25g butanone, stir 40min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5g defoamer solution, 0.2g promotor and 10g vinyl acetic monomer while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 110g Graphene and mix with 150g butanone, and add 1.1g coupling agent to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500r/min and within 5 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
3. a preparation method who contains the graphene conductive ink of 60g bisphenol A epoxide resin, is characterized in that, it comprises the following steps:
Get 60g bisphenol A epoxide resin and put into test bottle, add 25g butanone, stir 40min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5g defoamer solution, 0.2g promotor and 10g vinyl acetic monomer while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 300g Graphene and mix with 400g butanone, and add 3.0g coupling agent to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500r/min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
4. a preparation method who contains the graphene conductive ink of 60g bisphenol A epoxide resin, is characterized in that, it comprises the following steps:
Get 60g bisphenol A epoxide resin and put into test bottle, add 25g butanone, stir 40min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5g defoamer solution, 0.2g promotor and 10g vinyl acetic monomer while stirring in described mixed solution, in homogenizer, disperse 2 hours, obtain binder;
Take 300g Graphene and mix with 400g butanone, and add 3.0g coupling agent to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500r/min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
5. a preparation method who contains the graphene conductive ink of 60g bisphenol A epoxide resin, is characterized in that, it comprises the following steps:
Get 60g bisphenol A epoxide resin and put into test bottle, add 25g butanone, stir 40min until completely dissolved, add Dyhard RU 100-dimethyl formamide solution 11.0g to make mixed solution, this solution is fully dissolved in dimethyl formamide and makes by Dyhard RU 100, and wherein the ratio of Dyhard RU 100 and dimethyl formamide is 1:9, drips 1.5g defoamer solution, 0.2g promotor and 10g vinyl acetic monomer while stirring in described mixed solution, in homogenizer, disperse 1.5 hours, obtain binder;
Take 300g Graphene and mix with 400g butanone, and add 3.0g coupling agent to put into ultrasonic apparatus at 35 DEG C, to carry out ultrasonic dispersion with 2500r/min and within 8 hours, obtain graphene suspension, leave standstill and within 12 hours, isolate graphene solution;
In described binder, need under the condition stirring, add graphene solution, after adding, continue high-speed stirring 3 hours, after grinding, obtain graphene conductive ink.
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Effective date of registration: 20170704 Address after: 519000 No. 3199, South Avenue, Mount Everest, Zhuhai Town, Doumen District, Guangdong, China Patentee after: Zhuhai Letong New Material Science & Technology Co., Ltd. Address before: 519085 Guangdong city of Zhuhai province Jinding Leton Kwun Tong Industrial Park Patentee before: Letong Chemical Co., Ltd. |