CN106590177B - Graphene conductive ink and preparation method thereof - Google Patents
Graphene conductive ink and preparation method thereof Download PDFInfo
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- CN106590177B CN106590177B CN201611261271.8A CN201611261271A CN106590177B CN 106590177 B CN106590177 B CN 106590177B CN 201611261271 A CN201611261271 A CN 201611261271A CN 106590177 B CN106590177 B CN 106590177B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/104—Polyesters
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- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The present invention provides a kind of Graphene conductive inks, which is characterized in that by the gross mass of the Graphene conductive ink be 100% in terms of, the following component including following mass percentage: functionalization graphene 40-60%；Hyperbranched polycarbonates 20-30%；Fats bismaleimide 8-12%；Polyoxyethylene polyoxypropylene block ester copolymer 2-5%；Surplus is solvent；Wherein, the functionalization graphene is that the edge of graphene is connected with the graphene of polymethacrylates；The hyperbranched polycarbonates are the polycarbonate containing terminal hydroxyl, and the degree of branching of the hyperbranched polycarbonates is 0.35-0.52.
Description
Technical field
The invention belongs to electrically conductive ink fields more particularly to a kind of Graphene conductive ink and preparation method thereof.
Background technique
Electrically conductive ink is a kind of functional ink, usually by forming to point functional material and basis material.Wherein, conductive function
Energy material realizes conducting function by being dispersed in ink carrier, and existing conducting function material is mostly conductive metal powder, leads
Electrical carbon material；Basis material generally acts as binder and condiment ingredient, for adjusting the viscosity of ink or improving the machinery of ink
Support.There is electrically conductive ink that can be practical, including gold system electrically conductive ink, silver system electrically conductive ink, copper on the market at present
It is electrically conductive ink, carbon series conductive ink etc., is widely used in the fields such as printed circuit, electrode, electroplated layer.But with metal
Electrically conductive ink of the grain as raw material, it is not only expensive, but also needs be chemically synthesized, modify and separation and Extraction etc. more
Complicated preparation process.And carbon series conductive ink in the market, resistivity are higher, conductive effect is undesirable.
Graphene is carbon atom through sp2Hydridization and the two-dimension plane structure formed.Due to its two-dimentional conjugated structure, have excellent
Electric conductivity, heating conduction and stability more are a kind of good materials of application prospect.In recent years, graphene by
The concern of people is simultaneously widely studied, and the application based on graphene also emerges one after another.There is very strong mechanicalness as one kind
The material of energy and excellent electric conductivity energy (high conductivity), graphene have very strong application potential on electrically conductive ink field.
In electrically conductive ink, the addition of graphene compensates for the deficiency of metallic conductive inks, carbon series conductive ink to a certain extent, still,
Since graphene has great specific surface area, it is easy to happen reunion, therefore, existing Graphene conductive ink, electric conductivity
It can be there are also the very big rising space.
Summary of the invention
The purpose of the present invention is to provide a kind of Graphene conductive inks and preparation method thereof, it is intended to solve existing graphene
Electrically conductive ink is since graphene is easy to happen reunion, the problem of causing its electric conductivity that cannot effectively improve again.
The invention is realized in this way a kind of Graphene conductive ink, the gross mass with the Graphene conductive ink are
100% meter, the following component including following mass percentage:
Wherein, the functionalization graphene is that the edge of graphene is connected with the graphene of polymethacrylates；
The hyperbranched polycarbonates are the polycarbonate containing terminal hydroxyl, and the branching of the hyperbranched polycarbonates
Degree is 0.35-0.52.
Preferably, the fats bismaleimide is to have the following structure the fats bismaleimide of general formula:
Wherein, R1、R2、R3And R4It is selected from CH2(OH)(CH2)8OOCCH2-、CH3(CH2)12COOCH2(CH2)8CH2OOCCH2-、(CH3CH2CH2)2(CH2)8COOCH2CH(CH2CH3)CH2-、CH3CH2CH2COOCH2(CH2)11OOCCH2In
It is at least one.
It preferably, is the poly- first in terms of 100% by the gross weight of the functionalization graphene in the functionalization graphene
The mass percentage of base acrylate is 2-10%.
Preferably, the Graphene conductive ink further includes conductive auxiliary agent, and with total matter of the Graphene conductive ink
Amount is 100% meter, the content < 5% of the conductive auxiliary agent.
It is further preferred that the conductive auxiliary agent is at least one of nano-silver powder, copper nanoparticle, and the nano silver
Powder, copper nanoparticle partial size be 50-200nm.
Preferably, the hyperbranched polycarbonates and the mass ratio of the fats bismaleimide are 1:(0.3-
0.5)。
Preferably, the Graphene conductive ink further includes other auxiliary agents, other described auxiliary agents include stabilizer, thickening
At least one of agent, regulator, plasticizer, lubricant, inhibitor.
Preferably, the solvent is one or both of water, alcohols.
And a kind of preparation method of Graphene conductive ink, comprising the following steps:
Each component is weighed according to the formula of above-mentioned Graphene conductive ink；
Functionalization graphene, polyoxyethylene polyoxypropylene block ester copolymer and solvent are mixed, ultrasonic agitation point is passed through
It dissipates uniformly, reaches mixed liquor；
Hyperbranched polycarbonates and fats bismaleimide are added in the mixed liquor, is stirred by ultrasonic, at grinding
Reason, obtains Graphene conductive ink.
Preferably, the functionalization graphene is obtained by graphene and the organic matter progress ion exchange containing vinyl benzyl
It arrives.
Graphene conductive ink provided by the invention, using functionalization graphene as conductive filler, and the function fossil
Black alkene is that the edge of graphene is connected with the graphene of polymethacrylates, and not only described functionalization graphene itself can
Effectively improve the electric conductivity of Graphene conductive ink；And the functionalization graphene can reduce graphene agglomeration,
It is improved in the dispersion stabilization of ink system, further increases its electric conductivity.In addition, the functionalization graphene is compared with graphene
With better water-soluble and surface-active.Further, the present invention is with hyperbranched polycarbonates and fats bismaleimide
Amine is used as binder simultaneously, and the two cooperates, and forms the bonding system that adhesion strength is strong, stability is high, resistance variations are small, together
When, compound binding agent can effectively disperse the functionalization graphene, and it is substantially prevented between the functionalization graphene and reunites, from
And efficiently improve the electric conductivity of electrically conductive ink.In addition, the present invention uses polyoxyethylene polyoxypropylene block ester copolymer, it can be into
One step is cooperateed with above-mentioned bonding system, improves the dispersion stabilization of the functionalization graphene.To sum up, the present invention passes through triple anti-
Agglomeration techniques effectively reduce the reunion of graphene, finally obtain the electrically conductive ink that graphene dispersion state is excellent, electric conductivity is high.
Graphene conductive ink provided by the invention, only need to be fully dispersed uniformly by each component, and method is simple, is easy to
It realizes.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
The embodiment of the invention provides a kind of Graphene conductive ink, the gross mass with the Graphene conductive ink is
100% meter, the following component including following mass percentage:
Wherein, the functionalization graphene is that the edge of graphene is connected with the graphene of polymethacrylates；
The hyperbranched polycarbonates are the polycarbonate containing terminal hydroxyl, and the branching of the hyperbranched polycarbonates
Degree is 0.35-0.52.
In the embodiment of the present invention, using graphene as conductive filler, Lai Tigao ink electric conductivity.It is led since graphene is used as
It is easy to reunite when electric filler, the embodiment of the present invention is using functionalization graphene as conductive filler.Specifically, the function fossil
Black alkene is that the edge of graphene is connected with the graphene of polymethacrylates.It is repaired by the way that edge will be carried out to graphene sheet layer
Decorations processing introduces polymethacrylates in the edge of graphene, makes graphene planes charge, can not only improve
The storage modulus and conductivity of composite material；And its dispersibility can also be improved, reduce the agglomeration of functionalization graphene.This
Outside, the functionalization graphene also has preferable water-soluble, dispersion stabilization and surface-active, is conducive to improve electrically conductive ink
Comprehensive performance.
It is further preferred that being institute in terms of 100% by the gross weight of the functionalization graphene in the functionalization graphene
The mass percentage for stating polymethacrylates is 2-10%.The content of the polymethacrylates preferred scope, can
Preferably to avoid the reunion between graphene molecules.If the mass percentage of the polymethacrylates is too low, effect
It is unobvious；If the mass percentage of the polymethacrylates is excessively high, the graphene after will lead to functionalization loses it
Electrically conductive ink cannot be prepared under formulation condition of the embodiment of the present invention in the performance of script.It is furthermore preferred that the function fossil
It is in terms of 100% by the gross weight of the functionalization graphene, the mass percentage of the polymethacrylates is 3- in black alkene
5%.
As further preferred embodiments, conduction can be added in the Graphene conductive ink in the embodiment of the present invention and help
Agent, to meet the ink needs for having requirements at the higher level to electric conductivity.But it is with the gross mass of the Graphene conductive ink
100% meter, the content < 5% of the conductive auxiliary agent.If the adding too much of the conductive auxiliary agent can destroy implementation of the present invention
Example building dispersion, be unfavorable for ink performance raising,
It is further preferred that the conductive auxiliary agent is at least one of nano-silver powder, copper nanoparticle, and the nano silver
Powder, copper nanoparticle partial size be 50-200nm.The addition of the nano-silver powder, copper nanoparticle can make the function fossil
Black alkene is coated on its surface, forms core-shell structure, disperses with being conducive to the functionalization graphene not to the utmost, and can be to avoid
The reunion of nano particle itself.If the partial size of the nano-silver powder, copper nanoparticle is too small, the functionalization graphene can not be right
It is coated；If the partial size of the nano-silver powder, copper nanoparticle is excessive, it is unfavorable for the formation of conductive path.
In the embodiment of the present invention, in order to meet printing viscosity requirement, viscosity is added in the Graphene conductive ink
Regulator component.Specifically, viscosity modifier described in the embodiment of the present invention uses compound binding agent, the compound binding agent includes
Hyperbranched polycarbonates and fats bismaleimide.The compound binding agent has preferable rheological characteristic and film forming；Together
When also there is excellent adhesive force, resistance to acid and alkali and heat resistance.Importantly, the present invention is with hyperbranched polycarbonates and fat
Class bismaleimide is used as binder simultaneously, and the two cooperates, and formation adhesion strength is strong, stability is high, resistance variations are small
Bonding system, meanwhile, compound binding agent can effectively disperse the functionalization graphene, be substantially prevented from the functionalization graphene
Between reunite, thus efficiently improve electrically conductive ink electric conductivity.
Specifically, the hyperbranched polycarbonates are the polycarbonate containing terminal hydroxyl, and the hyperbranched poly carbonic acid
The degree of branching of ester is 0.35-0.52.If the esterification degree of the degree of branching of the hyperbranched polycarbonates is too low, hyper-branched polyester
Limited capacity；If the esterification degree of the degree of branching of the hyperbranched polycarbonates is excessively high, viscosity is excessive, is unfavorable for conductive filler
It is fully dispersed.
Preferably, the fats bismaleimide is to have the following structure the fats bismaleimide of general formula:
Wherein, R1、R2、R3And R4It is selected from CH2(OH)(CH2)8OOCCH2-、CH3(CH2)12COOCH2(CH2)8CH2OOCCH2-、(CH3CH2CH2)2(CH2)8COOCH2CH(CH2CH3)CH2-、CH3CH2CH2COOCH2(CH2)11OOCCH2In
It is at least one.
The fats bismaleimide of preferred structure, so that the bismaleimide has long-chain flexible, to make
The viscosity of the bismaleimide reduces, so that the hyperbranched polycarbonates be avoided to greatly improve viscosity.In addition, this hair
The interior high-temperature behavior of electrically conductive ink can be improved in the fats bismaleimide of bright embodiment preferred structure.Certainly, carbon carbon list
The quantity of key is not The more the better, if the quantity of carbon-carbon single bond is excessive, degree of cross linking increase will lead to flexible reduction instead.
It is further preferred that the hyperbranched polycarbonates and the mass ratio of the fats bismaleimide are 1:
(0.3-0.5), to realize preferable fiting effect.
The embodiment of the present invention using the polyoxyethylene polyoxypropylene block ester copolymer as dispersing agent, can further with
Above-mentioned bonding system collaboration, improves the dispersion stabilization of the functionalization graphene.
Solvent described in the embodiment of the present invention is one or both of water, alcohols.
In order to improve the comprehensive performance of electrically conductive ink, it is preferred that the Graphene conductive ink further includes other auxiliary agents, institute
Stating other auxiliary agents includes at least one of stabilizer, thickener, regulator, plasticizer, lubricant, inhibitor.
Graphene conductive ink provided in an embodiment of the present invention, using functionalization graphene as conductive filler, and the function
Energy graphite alkene is that the edge of graphene is connected with the graphene of polymethacrylates, not only the functionalization graphene sheet
Body can effectively improve the electric conductivity of Graphene conductive ink；And the functionalization graphene can reduce graphene reunion
Phenomenon improves it in the dispersion stabilization of ink system, further increases its electric conductivity.In addition, the functionalization graphene compared with
Graphene has preferably water-soluble and surface-active.Further, the embodiment of the present invention is with hyperbranched polycarbonates and fat
Class bismaleimide is used as binder simultaneously, and the two cooperates, and formation adhesion strength is strong, stability is high, resistance variations are small
Bonding system, meanwhile, compound binding agent can effectively disperse the functionalization graphene, be substantially prevented from the functionalization graphene
Between reunite, thus efficiently improve electrically conductive ink electric conductivity.In addition, the embodiment of the present invention uses polyoxyethylene polyoxypropylene
Block ester copolymer can be cooperateed with further with above-mentioned bonding system, improve the dispersion stabilization of the functionalization graphene.It is comprehensive
On, the embodiment of the present invention effectively reduces the reunion of graphene by triple anti-agglomeration technologies, finally obtains graphene dispersion state
Electrically conductive ink excellent, electric conductivity is high.
Graphene conductive ink provided in an embodiment of the present invention can be prepared by following methods.
And the embodiment of the invention also provides a kind of preparation methods of Graphene conductive ink, comprising the following steps:
S01. each component is weighed according to the formula of above-mentioned Graphene conductive ink；
Specifically, the recipe ingredient and its preferred situation of the Graphene conductive ink are as described above, in order to save a piece
Width, details are not described herein again.Wherein, it is preferred that the functionalization graphene passes through graphene and the organic matter containing vinyl benzyl
Ion exchange is carried out to obtain.
S02. functionalization graphene, polyoxyethylene polyoxypropylene block ester copolymer and solvent are mixed, is stirred by ultrasound
It mixes and is uniformly dispersed, reach mixed liquor；
By functionalization graphene, polyoxyethylene polyoxypropylene block ester copolymer and solvent mixed processing, the ultrasound is stirred
The time mixed is 2-8 hours.
S03. hyperbranched polycarbonates and fats bismaleimide are added in the mixed liquor, is stirred by ultrasonic, grinds
Mill processing, obtains Graphene conductive ink.
Binder hyperbranched polycarbonates and fats bismaleimide are added in the mixed liquor, is stirred through ultrasound
It mixes, Graphene conductive ink can be obtained in milled processed.Wherein, the time of the ultrasonic agitation is 2-8 hours, and grinding 2-5 is small
When.
Graphene conductive ink provided in an embodiment of the present invention, only need to be fully dispersed uniformly by each component, method letter
It is single, it is easy to accomplish.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of Graphene conductive ink, which is characterized in that by the gross mass of the Graphene conductive ink be 100% in terms of, packet
Include the following component of following mass percentage:
Wherein, the functionalization graphene is that the edge of graphene is connected with the graphene of polymethacrylates；
The hyperbranched polycarbonates are the polycarbonate containing terminal hydroxyl, and the degree of branching of the hyperbranched polycarbonates is
0.35-0.52；
The fats bismaleimide is to have the following structure the fats bismaleimide of general formula:
Wherein, R1、R2、R3And R4It is selected from CH2(OH)(CH2)8OOCCH2-、CH3(CH2)12COOCH2(CH2)8CH2OOCCH2-、
(CH3CH2CH2)2(CH2)8COOCH2CH(CH2CH3)CH2-、CH3CH2CH2COOCH2(CH2)11OOCCH2One of.
2. Graphene conductive ink as described in claim 1, which is characterized in that in the functionalization graphene, with the function
The gross weight of energy graphite alkene is 100% meter, and the mass percentage of the polymethacrylates is 2-10%.
3. Graphene conductive ink as described in claim 1, which is characterized in that the Graphene conductive ink further includes conduction
Auxiliary agent, and be the content < 5% of the conductive auxiliary agent in terms of 100% by the gross mass of the Graphene conductive ink.
4. Graphene conductive ink as claimed in claim 3, which is characterized in that the conductive auxiliary agent is nano-silver powder, nanometer
At least one of copper powder, and the partial size of the nano-silver powder, copper nanoparticle is 50-200nm.
5. Graphene conductive ink a method according to any one of claims 1-3, which is characterized in that the hyperbranched polycarbonates and institute
The mass ratio for stating fats bismaleimide is 1:(0.3-0.5).
6. Graphene conductive ink a method according to any one of claims 1-3, which is characterized in that the Graphene conductive ink is also wrapped
Include other auxiliary agents, other described auxiliary agents include stabilizer, thickener, regulator, plasticizer, lubricant, in inhibitor at least
It is a kind of.
7. Graphene conductive ink a method according to any one of claims 1-3, which is characterized in that the solvent is water, in alcohols
It is one or two kinds of.
8. a kind of preparation method of Graphene conductive ink, comprising the following steps:
Each component is weighed according to the formula of any Graphene conductive ink of claim 1-7；
Functionalization graphene, polyoxyethylene polyoxypropylene block ester copolymer and solvent are mixed, it is equal by ultrasonic agitation dispersion
It is even, reach mixed liquor；
Hyperbranched polycarbonates and fats bismaleimide are added in the mixed liquor, ultrasonic agitation, milled processed obtain
To Graphene conductive ink.
9. the preparation method of Graphene conductive ink as claimed in claim 8, which is characterized in that the functionalization graphene is logical
Graphene is crossed to obtain with the organic matter progress ion exchange containing vinyl benzyl.
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