CN109749518A - A kind of dilute electrically conductive ink of graphite and preparation method thereof - Google Patents
A kind of dilute electrically conductive ink of graphite and preparation method thereof Download PDFInfo
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- CN109749518A CN109749518A CN201711090434.5A CN201711090434A CN109749518A CN 109749518 A CN109749518 A CN 109749518A CN 201711090434 A CN201711090434 A CN 201711090434A CN 109749518 A CN109749518 A CN 109749518A
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Abstract
The present invention provides a kind of dilute electrically conductive ink composite material of graphite, and mainly matching (by mass percentage) includes 1 ~ 40 wt% of graphene；10 ~ 60 wt% of resin base connecting material；10 ~ 30 wt% of auxiliary agent etc..The experimental method provided according to the present invention can large batch of preparation Graphene conductive ink.The electrically conductive ink that the present invention obtains has high electrical conductivity, good toughness, pressing mold type energy and shock resistance.The present invention overcomes the pollution environment of conventional conductive ink and the drawbacks high at the present invention, are expected to large-scale commercial production.
Description
Technical field
The present invention relates to a kind of electrically conductive ink, especially a kind of Graphene conductive ink composite material and the electrically conductive ink
Preparation method.
Background technique
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made of carbon atom
Two dimensional crystal.2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao love, at
Function isolates graphene from graphite, it was demonstrated that therefore it can also obtain jointly 2010 years Nobel's physics with individualism, two people
Learn prize.Graphene is both most thin material, and most tough material, and 200 times more taller than best steel of breaking strength.Together
When it has good elasticity again, stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity is highest
Material.Graphene most potential application at present is the substitute as silicon, manufactures ultra micro transistor npn npn, for producing future
Supercomputer.Replace silicon with graphene, the speed of service of computer processor will be hundreds times fast.In addition, graphene is almost
It is fully transparent, the light of absorption 2.3%.On the other hand, it is very fine and close, even the smallest gas atom (helium atom)
Also it can not penetrate.These features make it be highly suitable as the raw material of transparent electron product, such as transparent touch display screen, hair
Tabula rasa and solar panel.As presently found most thin, maximum intensity, a kind of strongest novel nano of electrical and thermal conductivity performance
Material, graphene are referred to as " dark fund ", are " king of new material ", and scientist even foretells that graphene " will thoroughly change 21 generation
It records ".Very likely start the subversiveness new technology new industrial revolution have swept the globe.
With the fast development of electronics industry, electrically conductive ink is in flexible print circuit, thin film switch, radio frequency identification etc.
Application in field increasingly increases.Conductive filler is the key factor for determining electrically conductive ink electric conductivity, is classified by conductive filler,
Electrically conductive ink generally can be divided into carbon system, metal system and macromolecular.Carbon series conductive ink price is relatively inexpensive, but electric conductivity and moisture-proof
Property it is poor, be only used for conduction needs it is low product printing.Typical fillers in conventional carbon system electrically conductive ink include carbon black, stone
Ink and carbon fiber etc., conductivity change with the type of carbon and are changed, and there is low, the light, performance at the present invention to stablize, after solidification
The advantages that acid and alkali-resistance and chemical solvent corrosion, ink adhesion is strong.However, the electric conductivity of carbon black, graphite and carbon fiber without
Method meets the growth requirement of the following printed electronic industry.Conductive filler of the graphene as electrically conductive ink, not only electric conductivity is excellent
It is good, and have excellent corrosion resistance and inoxidizability, it is most to have one of printed electronic material of popularization and application potentiality.Graphite
Alkene electrically conductive ink is one of the hot spot of domestic and international graphene research field.
Summary of the invention
The present invention provides a kind of preparation cost invention it is low, electric conductivity is excellent, good mechanical property, component proportion is adjustable and
The Graphene conductive ink of ambient temperature curable, and its corresponding preparation method is provided.
The technical solution of the present invention is as follows:
Graphene conductive ink of the invention, the mass percent of ingredient are as follows: resin link stuff mass percent group is divided into 10 ~
60 wt%；Graphene mass percent group is divided into 1 ~ 40 wt%；Auxiliary agent mass percent group is divided into 10 ~ 30 wt%；Solvent quality
Percent composition is 5 ~ 80 wt%.
Resin in resin base connecting material according to the present invention can be natural resin, synthetic resin or modified tree
Rouge.Synthetic resin includes epoxy resin, phenolic resin, acrylic resin, polyvinyl fluoride, amide resin, heat in invention of the present invention
Mould plastics, synthetic cellulose, polyvinyl resin, synthetic rubber etc..It is available in invention of the present invention to have phenol-formaldehyde resin modified, modification
Epoxy resin, modified thermoplastic resin, modified cellulose and modified rubber.Above-mentioned resin is again main film forming matter in electrically conductive ink
Matter, physical and chemical performance will directly determine the bases such as mechanical property, rheological property, acid-proof alkaline, the adhesive force of electrically conductive ink
Plinth performance.
Graphene of the present invention includes that (number of plies is less than 10 for single-layer graphene, bilayer graphene and multi-layer graphene
Layer) and nano microcrystalline graphite alkene and the redox graphene being prepared using Hummers method.Graphene in the present invention
Particle size is about that 10nm or more thickness is about between 0.335nm to 1 microns, and shape can be sheet, threadiness, spherical
Deng.Above-mentioned graphene dominates the electric conductivity of finally obtained electrically conductive ink, so, the specific surface of graphene in electrically conductive graphite
Product is bigger, dispersion performance is better, and the electric conductivity of electrically conductive ink also can be better.
The present invention claims solvent be water, alcohol solvent, ketone solvent, ether solvent, hydrocarbon solvent, esters solvent and
Vegetable and animals oils and mineral oil.Solvent in the present invention mainly to the dissolution of resin and to conductive compositions graphene and auxiliary agent into
Row peptizaiton.Furthermore dissolution also determines the viscosity and rate of drying of electrically conductive ink.
Auxiliary agent used in the present invention include thickener, dispersing agent, coupling agent, plasticizer, advection agent, colorant, lubricant,
Stabilizer, antioxidant etc..The auxiliary agent of the present invention is ink area common agents, and main function is the steady of raising ink
Qualitative and printing performance, part of auxiliary also can be improved appropriately and be promoted to electrically conductive ink electric conductivity.For example, thickener can
To be used to improve the viscosity of electrocondution slurry, simultaneously dispersing solid particles are covered, prevent solid particle from reuniting.In addition, it can also change
Become the effect of the viscosity of electrically conductive ink.
The conductivity according to required for electrically conductive ink, viscosity, rheological characteristic, mode of printing in the present invention, the items such as substrate
The selection and adjusting of part progress resin connecting material, the component ratio of solvent, promoter material.
The present invention provides the preparation method of above-mentioned Graphene conductive ink composite material, mainly includes four steps:
1. weighing raw material: weighing each component material, each component according to the mass percent component of Graphene conductive ink
The specific mass ratio of material can be regulated and controled according to performance requirements such as the conductivities, viscosity, rheological characteristic of electrically conductive ink；
2. mixing: each load weighted material being imported in Scattered Kettle and is stirred at room temperature with the speed of 100 ~ 5000 rpm, is each
The dispersion of a component material, which is adjusted, to be mixed even, obtains electrically conductive ink slurry；Mixing speed in Scattered Kettle depends on the grain of initial component
Situations such as degree, shape and uniformity of dispersion.
3. grinding: obtained electrically conductive ink slurry is ground using grinder, grinding duration according to pulp components and
Initial particle size, shape can differ for -150 hours 1 hour；
4. grinding product is filtered, enfeoffment packaging obtains commercially available Graphene conductive ink.
Each raw material, component, auxiliary agent, solvent and processing method are not to electrically conductive ink composite material in the present invention
Limitation, but the features of the present invention.Firstly, the electrically conductive ink of system of the present invention, with low constituent content and electric conductivity it is excellent
Graphene dispersion is mutually conductive phase, and matrix phase is constituted using resin-based materials as connecting material, using auxiliary agent and solvent as auxiliary material, is led to
The regulation of component is crossed to change the viscosity and rheological characteristic of electrically conductive ink, and mechanical performance to electrically conductive ink and printing performance, with
And its resistance to acid and alkali can be carried out regulation, be finally reached the expected using effect of electrically conductive ink.Secondly, with graphene in the present invention
This product density is enabled to reduce while reducing filler share instead of traditional nano metal powder, resistance to settling mentions
Height, electrical conductivity are also greatly improved.In addition, graphene-based carbon filler its property is stable, antioxygenic property is good,
The pollution problem of heavy metal nanoparticle is also avoided on the basis of stable mechanical performance.Finally, being led based on this two dimension of graphene
The excellent mechanical flexibility of electric material can be with big specific surface area, good, flexible, the anti-stripping of conductive ink material flexibility obtained
The advantages that good from performance.
Graphene conductive ink produced by the present invention is suitable for brushing, screen printing rinses buckplate printing, spraying, offset printing, soft
Property version printing and volume print (roll to roll) etc. techniques, substrate can be paper, glass, ceramics, plastics, rubber, fibre
Dimension, cloth etc..
The electrically conductive ink room temperature curing time of the invention is less than 0.01-24 hours；The temperature range that is heating and curing is 30-200
DEG C, the time is 0.01-12 hours；Sintering curing temperature is 100-1000 DEG C, and the time is 0.01-12 hours.
Electrically conductive ink electric conductivity produced by the present invention is excellent, and printing adaptability is good, condition of cure is mild and low in cost,
It can be widely applied to thin film switch, transparent conductive film, plasma scope, flexible circuit board, circuit board, chemistry or biology to pass
The frivolous electronic product such as sensor, light emitting diode and flexible electronic product have vast potential market.
Specific embodiment:
To better understand the objects, features and advantages of the present invention, being done below with reference to embodiment to the present invention
It further illustrates.It should be noted that in the absence of conflict, the feature in embodiments herein and embodiment can phase
Mutually combination.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to the specific of specification is described below
The limitation of embodiment.
Example 1. weighs 40 parts of phenolic resin, and 20 parts of graphene, 25 parts of glycerine, 20 parts of dimethylbenzene, 2 parts of polyacrylic acid uranium salt,
It 2 parts of fatty acid ester sulfate, 2 parts of polysiloxane defoamer, 2 parts of dimethyl silicone polymer, 2 parts of polyurethane rheological agent, is put into
It stirs, be uniformly mixed in Scattered Kettle, obtain pre-dispersed material；Obtained pre-dispersed material is transferred in grinder until fineness of materials
Reach 10 microns or less；By ground material filtering, Graphene conductive ink can be obtained.
Example 2. weighs 30 parts of bisphenol A epoxide resin, and 10 parts of ethylene glycol, 20 parts of dimethylbenzene, 5 parts of triethylamine, polycarboxylate sodium 1
Part, 1 part of fatty vinegar sulfate, 1 part of polysiloxane defoamer, 1 part of dimethyl silicone polymer, association type acrylate 1
Part, it 30 parts of redox graphene, is put into stirring in Scattered Kettle, is uniformly mixed, obtain pre-dispersed material；It is pre-dispersed by what is obtained
Material, which is transferred in grinder, to be ground, until fineness of materials reaches 10 microns or less；By ground material filtering, stone can be obtained
Black alkene electrically conductive ink.
Graphene obtained above is received into electrically conductive ink using PET plastic film as substrate, using the halftone of 200 mesh, carries out silk
Wire mark brush, then it is dried at room temperature for solidification 20min, the cured composite conducting ink film with a thickness of 10 μm or so is finally obtained,
It is tested, as a result as follows:
The graphene ink that the present embodiment uses high-speed inkjet printer to prepare Examples 1 and 2, carries out printing smooth performance
Test.Wherein, test temperature is 25 DEG C, testing humidity 75%, and specific test result is as follows shown in table:
In conclusion the graphene ink of the embodiment of the present invention, can be filled into phenol for the graphene with excellent conductive performance
In urea formaldehyde or epoxy resin paste system, and it is well dispersed.Graphene layer imparts the good electric conductivity of solidify coating
And mechanical stability.The excellent characteristics such as resin material flexibility is good, caking property is good, weather-proof color inhibition, refractive index height, can be comprehensive
Meet and applies performance requirements.Whole preparation process of the present invention is controllable, easy to operate, low in cost, solvent-free volatilization, environment
Close friend is suitble to large-scale industrial production.
Claims (6)
1. a kind of Graphene conductive ink, the mass percent of ingredient are as follows: resin link stuff mass percent group be divided into 10 to
60 wt%；Graphene mass percent group is divided into 1 to 40 wt%；Auxiliary agent mass percent group is divided into 10 to 30 wt%；Solvent matter
Amount percent composition is 5 to 80 wt%.
2. the resin in resin base connecting material according to the present invention can be natural resin, synthetic resin or modified resin；
Synthetic resin is a kind of artificial synthesized a kind of heavy polymer, is had both or more than the one of natural resin inherent characteristic
Kind resin；Synthetic resin includes epoxy resin, phenolic resin, acrylic resin, polyvinyl fluoride, amide tree in invention of the present invention
Rouge, thermoplastic, synthetic cellulose, polyvinyl resin, synthetic rubber etc.；Modified resin is in general-purpose plastics and engineering plastics
On the basis of, by the methods of filling, enhancing processing, improve the performance of anti-flammability, intensity, impact resistance, toughness etc.
Plastic products；It is available in invention of the present invention to have phenol-formaldehyde resin modified, modified epoxy, modified thermoplastic resin, modified fibre
Element and modified rubber.
3. graphene of the present invention includes single-layer graphene, bilayer graphene and multi-layer graphene (number of plies is less than 10 layers)
And the redox graphene that nano microcrystalline graphite alkene and use Hummers method are prepared；The grain of graphene in the present invention
Diameter size is about that 10nm or more thickness is about between 0.335nm to 1 microns, and shape can be sheet, threadiness, spherical etc..
4. the present invention claims solvent be water, alcohol solvent, ketone solvent, ether solvent, hydrocarbon solvent, esters solvent and dynamic
Vegetable oil and mineral oil.
5. auxiliary agent used in the present invention includes thickener, dispersing agent, coupling agent, plasticizer, advection agent, colorant, lubricant, steady
Determine agent, antioxidant etc..
6. the preparation method of the Graphene conductive ink is main are as follows: 1. weigh raw material: according to the quality of Graphene conductive ink
Percent composition weighs each component material；2. mixing: each load weighted material is imported in Scattered Kettle with 100 ~ 5000
The speed of rpm is stirred at room temperature, and is that the dispersion of each component material adjusts and is mixed even, obtains electrically conductive ink slurry；3. grinding: using and grind
Grinding machine grinds obtained electrically conductive ink slurry, and grinding duration can be differed according to pulp components for -150 hours 1 hour；④
Grinding product is filtered and obtains commercially available Graphene conductive ink.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711090434.5A CN109749518A (en) | 2017-11-08 | 2017-11-08 | A kind of dilute electrically conductive ink of graphite and preparation method thereof |
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| CN201711090434.5A CN109749518A (en) | 2017-11-08 | 2017-11-08 | A kind of dilute electrically conductive ink of graphite and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410871A (en) * | 2020-03-06 | 2020-07-14 | 南昌欧菲生物识别技术有限公司 | Conductive ink, display module and electronic equipment |
| CH719589A1 (en) * | 2022-04-12 | 2023-10-31 | Graphenaton Tech Sa | Ink containing graphene. |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113786A (en) * | 2013-03-07 | 2013-05-22 | 苏州牛剑新材料有限公司 | Graphene conductive ink and preparation method thereof |
| CN103834235A (en) * | 2014-02-20 | 2014-06-04 | 江苏格美高科技发展有限公司 | Conductive graphene carbon slurry printing ink and preparation method thereof |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103113786A (en) * | 2013-03-07 | 2013-05-22 | 苏州牛剑新材料有限公司 | Graphene conductive ink and preparation method thereof |
| CN103834235A (en) * | 2014-02-20 | 2014-06-04 | 江苏格美高科技发展有限公司 | Conductive graphene carbon slurry printing ink and preparation method thereof |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410871A (en) * | 2020-03-06 | 2020-07-14 | 南昌欧菲生物识别技术有限公司 | Conductive ink, display module and electronic equipment |
| CH719589A1 (en) * | 2022-04-12 | 2023-10-31 | Graphenaton Tech Sa | Ink containing graphene. |
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Address after: Room 303b, Xinye building, Pioneer Park, torch hi tech Zone, Xiamen, Fujian, 361000 Applicant after: XIAMEN TEKILIFI ELECTRONIC TECHNOLOGY Co.,Ltd. Applicant after: XIAMEN TEKI GUANGHUI NEW MATERIAL Co.,Ltd. Address before: Room 303b, Xinye building, Pioneer Park, torch hi tech Zone, Xiamen City, Fujian Province Applicant before: XIAMEN TAIQILIFEI ELECTRONIC TECHNOLOGY Co.,Ltd. Applicant before: XIAMEN TEKI GUANGHUI NEW MATERIAL Co.,Ltd. |
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Application publication date: 20190514 |
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