CN103834235A - Conductive graphene carbon slurry printing ink and preparation method thereof - Google Patents
Conductive graphene carbon slurry printing ink and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a conductive graphene carbon slurry printing ink and a preparation method thereof; the printing ink comprises a conductive function unit containing graphene, solvent, auxiliary agent and resin bridging agent; the components comprise 10-70 parts of conductive units by weight, 10-90 parts of solvent by weight, 0.1-30 parts of auxiliary agent by weight, and 0-70 parts of resin bridging agent by weight. The preparation method comprises the preparation of conductive unit dispersion liquid and the preparation of conductive slurry. The preparation method of the conductive graphene carbon slurry printing ink is simple in method; compared with the conventional carbon slurry, the conductive graphene carbon slurry printing ink is high in conductivity, thin, uniform and smooth in printing film, excellent in performance, and is suitable for many printing technology and base materials.
Description
Technical field
The present invention relates to a kind of electrically conductive ink, particularly a kind of preparation method of electrically conductive graphite olefinic carbon paste printing ink.
Background technology
Electrically conductive ink refers to and is printed on stock, the ink that makes it to there is conduction current and get rid of accumulate static charge ability, it is the critical material in printed wiring, intelligent label, flexible display device, sensor printed electronics technology, the raising of electrically conductive ink performance, will promote the development of electronic industry, the development of electronics technology simultaneously is also had higher requirement to electrically conductive ink, and improving performance, reducing costs is the target that electrically conductive ink is constantly pursued.
Traditional electrically conductive ink is substantially added in polymkeric substance and is composited by conductive unit powder, and conducting function unit is the component of most critical, mainly contains carbon, metal or metal oxide and mixture three major types.Gold and silver and copper paste printing ink have good electroconductibility, and resistance value can reach 10
-2~10
-3Ω cm; Gold and silver ink performance is good, but expensive, and silver self exists the defects such as easy migration, sulfuration, anti-scolding tin etch ability, the easy cracking of sintering process.Copper paste printing ink can produce zone of oxidation under empty G&W effect makes electroconductibility unstable.Carbon paste printing ink rete is not oxidizable, stable performance, and acid-and base-resisting and chemical solvents corrosion after solidifying, the strong adhesion of ink, but resistivity is lower, is generally 10
2~10
-1Ω cm.Metal current and traditional carbon paste printing ink all exist the relative merits of self, and for improving performance, the improvement of conducting function unit and the new conductive unit of exploration application are the development trends of at present domestic and international electrically conductive ink research.
Graphene is the nano-carbon material of new generation of Geim group report in 2004, is a kind of carbon atom is honeycomb crystal lattice flat film with sp2 hybridized orbital composition hexangle type.Under normal temperature, its electronic mobility exceedes 1.5 × 104cm2/Vs, and than CNT (carbon nano-tube) or silicon wafer height, and only about 10-6 Ω cm of resistivity is lower than copper or silver, is the current material of resistivity minimum in the world.The feature such as stability and nano-lamellar structure of high conductivity, carbon material essence has all determined that Graphene can be used as high-quality electrically conductive ink functional unit and prepares Graphene ink.
Be different from metal, Graphene does electro-conductive material and has lamellar interface resistance.In addition, because oxide-reduction method raw material is the abundant graphite in source, be one of method of large-scale low-cost industrialization Graphene, but there is textural defect in Graphene prepared by oxide-reduction method.Interface resistance and textural defect all cause the actual electroconductibility of graphene conductive material and the theoretical electroconductibility of Graphene to have a long way to go, and simple Graphene product application is expensive.Chinese invention patent 201310073034.9 discloses a kind of graphene conductive ink and preparation method thereof, and ink component comprises resin, Graphene, auxiliary agent and solvent.This ink adopts independent Graphene to do ink conductive unit, and therefore cost is high.Introduce and do conducting function unit with the mode part of hydridization, improving performance and reducing costs is the effective means that promotes the application of Graphene ink.Chinese invention patent 201210592284.9 discloses a kind of graphene-based electrically conductive ink, its preparation method and compliant conductive film; ink component comprises resin, conducting function unit, solvent and auxiliary agent, and wherein conducting function unit is made up of a kind of carbon material in Graphene and carbon black and the carbon nanotube of loaded metal particle or tinsel.
Summary of the invention
The object of the present invention is to provide a kind of electrically conductive graphite olefinic carbon slurry, solve the with high costs and conventional carbon of simple Graphene ink slurry electroconductibility low technical problem, this electrically conductive ink is reducing under the prerequisite of simple Graphene ink cost, and electroconductibility obviously improves with respect to conventional carbon slurry.
The present invention also aims to provide a kind of electrically conductive graphite olefinic carbon paste printing ink that prints high quality circuit and be suitable for multiple typography, the rete being printed by this electrically conductive ink is thin and uniform and smooth, excellent property; In addition, this electrically conductive ink is except being applicable to traditional typography, also can modulate and be applicable to ink-jet, directly write contour smart typography.
The object of the invention is to be achieved through the following technical solutions, a kind of electrically conductive graphite olefinic carbon paste printing ink, this ink comprises conducting function unit, solvent, auxiliary agent and the resin linking agent of graphene-containing, and each component consists of according to parts by weight: conductive unit is 10-70 part; Solvent is 10-90 part; Auxiliary agent is 0.1-30 part; Resin linking agent is 0-70 part.
As optimization: the conducting function unit of described graphene-containing is made up of Graphene and other conductive carbon nuclear matter, Graphene and other conductive carbon nuclear matter mass ratio are 1: 0.1~1: 100.
As optimization: other described conductive carbon nuclear matter comprises one or several in graphite, conductive channel black, acetylene black, furnace treated black, carbon fiber, carbon crystalline substance.
As optimization: described solvent comprises one or several in water, fat hydrocarbon solvent, aromatic hydrocarbon solvent, alcoholic solvent, ketones solvent, esters solvent, alcohol ether solvent, animal oils, mineral oil.
As optimization: described auxiliary agent comprises one or several in dispersion agent, stablizer, protective material, membrane-forming agent, coupling agent, softening agent, defoamer, thickening material, wetting agent, flow agent, thixotropic agent, linking agent, sterilant, light trigger, thermal initiator, uv-absorbing agent.
As optimization: described resin linking agent is the modified resin of natural resin, synthetic resins and natural and synthetic resins.
As optimization: described natural resin comprises: rosin, amber, shellac; Described synthetic resins comprises: epoxy resin, resol, vibrin, silicone resin, fluorocarbon resin, unsaturated polyester resin, acrylic resin, acrylate quasi-oligomer and reactive monomer, Synolac, Vinylite, synthetic cellulose, polyamide resin, vinyl chloride-vinyl acetate resin, urethane resin, polyvinylidene fluoride resin, thermoplastic resin, synthetic rubber; Described modified resin comprises: polyurethane modified epoxy, silicon-modified epoxy, organosilicon-modified acrylic epoxy resin, modified phenolic, acrylic resin modified, modified alkyd resin, wax and modified rosin resin or its multipolymer.
As optimization: the lamella of described Graphene is of a size of 0.3-1 × 10
4nm, lamella is individual layer, bilayer or multilayer.
A preparation method for electrically conductive graphite olefinic carbon paste printing ink, comprises following preparation process:
(1) conductive unit dispersion liquid preparation
Weigh Graphene and other conductive carbon nuclear matter according to parts by weight, with solvent and dispersant, and by stirring 0.5~6h, ultrasonic 0.5~12h, grind 0.5~12h and be uniformly dispersed, make conductive unit dispersion liquid;
(2) preparation of electrocondution slurry
Form conductive unit dispersion liquid and solvent, auxiliary agent and mixed with resin according to electrically conductive ink, and by stir 0.5~6h, ultrasonic 0.5~12h, grind 0.5~12h slurry is mixed, obtain electrically conductive graphite olefinic carbon paste printing ink through test package.
Prepare electrically conductive graphite olefinic carbon slurry provided by the invention and comprise above conducting function unit, solvent, auxiliary agent, resin and preparation process, but should be understood to, these are described is in order to further illustrate the features and advantages of the present invention, instead of the restriction that the present invention is required.
Beneficial effect: the invention provides a kind of electrically conductive graphite olefinic carbon slurry and preparation method thereof, this conductive carbon paste advantage is: conductivity improves compared with conventional carbon slurry, and the addition of the identical required conductive unit of electroconductibility reduces; Graphene add-on is few, and more simple graphene conductive ink cost is low.In addition, adding of conductive nano unit, makes to print rete thin and uniform and smooth, excellent property, and this also saves material in a large number, and the minimizing of particle has also determined that this electrically conductive ink is suitable for meticulous undersized circuit printing.
Electrically conductive graphite olefinic carbon provided by the invention is starched outstanding feature:
(1) physical properties such as electrically conductive graphite olefinic carbon provided by the present invention slurry solid content, surface tension and viscosity can regulate as required, and applicable printing element and typography are extensive.As be applicable to the multiple base materials such as glass, pottery, metal, semi-conductor, rubber, plastics, paper, fiber, and be applicable to the traditional printing of offset printing, intaglio plate, letterpress and silk-screen, also be applicable to spraying, dip-coating etc., also can modulate and be applicable to volume to volume, ink-jet, directly the technique such as write.
(2) adding of conductive nano unit, makes to print rete thin and uniform and smooth, excellent property, and this also saves material in a large number, and the minimizing of particle has also determined that this electrically conductive ink is suitable for meticulous undersized circuit printing.
(3) conductivity improves compared with conventional carbon slurry, and the addition of the identical required conductive unit of electroconductibility reduces, and makes performance and cost obtain optimization.
(4) corrosion of not oxidizable, the stable performance of printed matter, acid and alkali-resistance and chemical solvents.
Embodiment:
Embodiment: embodiment is below to further illustrate of the present invention, instead of limits the scope of the invention.
Summary, a kind of electrically conductive graphite olefinic carbon paste printing ink, this ink comprises conducting function unit, solvent, auxiliary agent and the resin linking agent of graphene-containing.
The conducting function unit of graphene-containing is made up of Graphene and other conductive carbon nuclear matter.Other conductive carbon nuclear matter comprises one or several in graphite, conductive channel black, acetylene black, furnace treated black, carbon fiber, carbon crystalline substance.
Solvent comprises one or several in water, fat hydrocarbon solvent, aromatic hydrocarbon solvent, alcoholic solvent, ketones solvent, esters solvent, alcohol ether solvent, animal oils, mineral oil.
Auxiliary agent comprises one or several in dispersion agent, stablizer, protective material, membrane-forming agent, coupling agent, softening agent, defoamer, thickening material, wetting agent, flow agent, thixotropic agent, linking agent, sterilant, light trigger, thermal initiator, uv-absorbing agent.
Resin linking agent is the modified resin of natural resin, synthetic resins and natural and synthetic resins.Described natural resin comprises: rosin, amber, shellac; Described synthetic resins comprises: epoxy resin, resol, vibrin, silicone resin, fluorocarbon resin, unsaturated polyester resin, acrylic resin, acrylate quasi-oligomer and reactive monomer, Synolac, Vinylite, synthetic cellulose, polyamide resin, vinyl chloride-vinyl acetate resin, urethane resin, polyvinylidene fluoride resin, thermoplastic resin, synthetic rubber; Described modified resin comprises: polyurethane modified epoxy, silicon-modified epoxy, organosilicon-modified acrylic epoxy resin, modified phenolic, acrylic resin modified, modified alkyd resin, wax and modified rosin resin or its multipolymer.
The preparation method of Graphene comprises: the methods such as oxide-reduction method, chemical gaseous phase depositing process, solution stripping means, solvent thermal, high temperature reduction, electrochemistry and microwave.The lamella of Graphene is of a size of 0.3-1 × 10
4nm, lamella is individual layer, bilayer or multilayer.
Embodiment 1
A kind of electrically conductive graphite olefinic carbon paste printing ink, this ink comprises conducting function unit, solvent, the auxiliary agent of graphene-containing, each component consists of according to parts by weight: conductive unit is 10 parts; Solvent is 10 parts; Auxiliary agent is 0.1 part.
A preparation method for electrically conductive graphite olefinic carbon paste printing ink, comprises following preparation process:
(1) conductive unit dispersion liquid preparation
Weigh Graphene and other conductive carbon nuclear matter according to parts by weight, with solvent and dispersant, and be uniformly dispersed by stirring 0.5h, ultrasonic 0.5h, grinding 0.5h, make conductive unit dispersion liquid;
(2) preparation of electrocondution slurry
According to electrically conductive ink composition, conductive unit dispersion liquid is mixed with solvent, auxiliary agent, and by stirring 0.5h, ultrasonic 0.5h, grinding 0.5h, slurry is mixed, obtain electrically conductive graphite olefinic carbon paste printing ink through test package.
Embodiment 2
A kind of electrically conductive graphite olefinic carbon paste printing ink, this ink comprises conducting function unit, solvent, auxiliary agent and the resin linking agent of graphene-containing, each component consists of according to parts by weight: conductive unit is 70 parts; Solvent is 90 parts; Auxiliary agent is 30 parts; Resin linking agent is 70 parts.
A preparation method for electrically conductive graphite olefinic carbon paste printing ink, comprises following preparation process:
(1) conductive unit dispersion liquid preparation
Weigh Graphene and other conductive carbon nuclear matter according to parts by weight, with solvent and dispersant, and be uniformly dispersed by stirring 6h, ultrasonic 12h, grinding 12h, make conductive unit dispersion liquid;
(2) preparation of electrocondution slurry
Form conductive unit dispersion liquid and solvent, auxiliary agent and mixed with resin according to electrically conductive ink, and by stirring 6h, ultrasonic 12h, grinding 12h, slurry is mixed, obtain electrically conductive graphite olefinic carbon paste printing ink through test package.
Embodiment 3
A kind of electrically conductive graphite olefinic carbon paste printing ink, this ink comprises conducting function unit, solvent, auxiliary agent and the resin linking agent of graphene-containing, each component consists of according to parts by weight: conductive unit is 38 parts; Solvent is 49 parts; Auxiliary agent is 22 parts; Resin linking agent is 61 parts.
A preparation method for electrically conductive graphite olefinic carbon paste printing ink, comprises following preparation process:
(1) conductive unit dispersion liquid preparation
Weigh Graphene and other conductive carbon nuclear matter according to parts by weight, with solvent and dispersant, and be uniformly dispersed by stirring 4h, ultrasonic 7h, grinding 9h, make conductive unit dispersion liquid;
(2) preparation of electrocondution slurry
Form conductive unit dispersion liquid and solvent, auxiliary agent and mixed with resin according to electrically conductive ink, and by stirring 3h, ultrasonic 8h, grinding 9h, slurry is mixed, obtain electrically conductive graphite olefinic carbon paste printing ink through test package.
Claims (9)
1. an electrically conductive graphite olefinic carbon paste printing ink, is characterized in that: this ink comprises conducting function unit, solvent, auxiliary agent and the resin linking agent of graphene-containing, and each component consists of according to parts by weight: conductive unit is 10-70 part; Solvent is 10-90 part; Auxiliary agent is 0.1-30 part; Resin linking agent is 0-70 part.
2. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 1, is characterized in that: the conducting function unit of described graphene-containing is made up of Graphene and other conductive carbon nuclear matter, and Graphene and other conductive carbon nuclear matter mass ratio are 1: 0.1~1: 100.
3. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 2, is characterized in that: other described conductive carbon nuclear matter comprises one or several in graphite, conductive channel black, acetylene black, furnace treated black, carbon fiber, carbon crystalline substance.
4. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 1, is characterized in that: described solvent comprises one or several in water, fat hydrocarbon solvent, aromatic hydrocarbon solvent, alcoholic solvent, ketones solvent, esters solvent, alcohol ether solvent, animal oils, mineral oil.
5. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 1, is characterized in that: described auxiliary agent comprises one or several in dispersion agent, stablizer, protective material, membrane-forming agent, coupling agent, softening agent, defoamer, thickening material, wetting agent, flow agent, thixotropic agent, linking agent, sterilant, light trigger, thermal initiator, uv-absorbing agent.
6. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 1, is characterized in that: described resin linking agent is the modified resin of natural resin, synthetic resins and natural and synthetic resins.
7. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 6, is characterized in that: described natural resin comprises: rosin, amber, shellac; Described synthetic resins comprises: epoxy resin, resol, vibrin, silicone resin, fluorocarbon resin, unsaturated polyester resin, acrylic resin, acrylate quasi-oligomer and reactive monomer, Synolac, Vinylite, synthetic cellulose, polyamide resin, vinyl chloride-vinyl acetate resin, urethane resin, polyvinylidene fluoride resin, thermoplastic resin, synthetic rubber; Described modified resin comprises: polyurethane modified epoxy, silicon-modified epoxy, organosilicon-modified acrylic epoxy resin, modified phenolic, acrylic resin modified, modified alkyd resin, wax and modified rosin resin or its multipolymer.
8. electrically conductive graphite olefinic carbon paste printing ink as claimed in claim 1, is characterized in that: the lamella of described Graphene is of a size of 0.3-1 × 10
4nm, lamella is individual layer, bilayer or multilayer.
9. a preparation method for electrically conductive graphite olefinic carbon paste printing ink, is characterized in that: comprise following preparation process:
(1) conductive unit dispersion liquid preparation
Weigh Graphene and other conductive carbon nuclear matter according to parts by weight, with solvent and dispersant, and by stirring 0.5~6h, ultrasonic 0.5~12h, grind 0.5~12h and be uniformly dispersed, make conductive unit dispersion liquid;
(2) preparation of electrocondution slurry
Form conductive unit dispersion liquid and solvent, auxiliary agent and mixed with resin according to electrically conductive ink, and by stir 0.5~6h, ultrasonic 0.5~12h, grind 0.5~12h slurry is mixed, obtain electrically conductive graphite olefinic carbon paste printing ink through test package.
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