CN108530996A - A kind of one-step method prepares graphene-based water-soluble conducting ink and preparation method thereof - Google Patents
A kind of one-step method prepares graphene-based water-soluble conducting ink and preparation method thereof Download PDFInfo
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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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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Abstract
The present invention relates to a kind of one-step method to prepare graphene-based water-soluble conducting ink and preparation method thereof, i.e.,：1 ~ 8 part of expanded graphite, 10 ~ 30 parts of conductive fillers, 10 ~ 50 parts of water-soluble resins, 20 ~ 80 parts of solvents and 1 ~ 10 part of auxiliary agent are added to together in high pressure homogenizer and carries out high shear and is ground to slurry granularity less than 80 μm, you can obtains graphene-based electrically conductive ink that is conductive excellent and having good stability.During shearing grinding, stripping and conducting particles to expanded graphite carry out intercalation between graphite flake layer and are completed at the same time this method, to establish complete good conductive network.This method is easy to operate, time-consuming short, avoids the stacking between graphene sheet layer and without abrasive media, subsequent processing is simple, be suitable for production.Prepared graphene-based water-soluble conducting ink is scattered, and stability is high.
Description
Technical field
The invention belongs to technical field of electronic materials, and graphene-based waterborne conductive oil is prepared more particularly to a kind of one-step method
Ink and preparation method thereof.
Background technology
Electrically conductive ink be it is a kind of be made of conductive filler, binder, solvent and auxiliary agent, there is electric conductivity to a certain degree
The paste-like ink of matter, is commonly called as paste ink.Wherein, conductive filler is the main ingredient for determining electrically conductive ink electric conductivity.Stone
Black alkene has many unique physical chemistry as individual layer laminated structure two dimension carbon material that is of new generation, being made of carbon atom
Property, theoretical specific surface area is up to 2600m2/ g, conductivity are up to 1250 ~ 7000s/m；In addition, graphene is also with excellent
Light transmission and good mechanical performance and thermodynamic stability are a kind of good electrically conductive ink fillers.
However, since the stronger Van der Waals force of piece interlayer makes graphene easily stack, specific surface area substantially reduces, whole
Electric conductivity and stability reduce.Graphene is modified, dispersibility of the graphene in aqueous solution and water-base resin is improved
Become research hotspot in recent years with stability.At present using more modified graphene slurry be mostly nitrogen-doped graphene,
Phosphorus doping graphene, boron doping graphene and polyaniline/polypyrrole modified graphene, above-mentioned modified graphene is to a certain degree
On enhance the dispersibility of graphene in aqueous solution, but preparation process is complicated and long-term storage will appear irreversible reunion and heavy
Lamination drops, and it is uneven with the compound batch mixing of other materials and cannot store for a long time.
Patent CN107298901A has invented a kind of carbon series conductive ink, is raw material with expanded graphite, and dry ball milling 0.1 ~
10h obtains graphene presoma, is then mixed with other conductive fillers, the binder mixed liquor of premixing and auxiliary agent and continues ball
0.5 ~ 50h is ground, electrically conductive ink is prepared.The invention simplifies dispersion and the stripping technology of graphene, is preparing electrically conductive ink
During simultaneously stripping obtained graphite microchip or graphene, but the preparation method complex process, take it is longer and need borrow
Assistant research fellow's grinding media, whole production cost is higher, is unsuitable for a large amount of outputs.
Invention content
The present invention is in view of the above-mentioned problems, provide the preparation side that a kind of one-step method prepares graphene-based water-soluble conducting ink
Method, technical scheme is as follows：
A) each raw material is weighed by mass component ratio, wherein solvent weighs under the conditions of being protected from light；
B) under the conditions of being protected from light, solvent, expanded graphite, water-soluble resin, conductive filler and auxiliary agent are added to high pressure together
High shear grinding is carried out in homogenizer.It is 207Mpa that high pressure homogenizer, which is used maximum pressure, you can obtains watersoluble plumbago alkene and changes
Property electrically conductive ink.
Wherein, step a) material qualities group is divided into：1 ~ 8 part of expanded graphite, 10 ~ 30 parts of conductive filler, water-soluble resin 10
1 ~ 10 part of ~ 50 parts, 20 ~ 80 parts of solvent and auxiliary agent.
Conducting particles in the conductive filler includes superconduction carbon black, acetylene black, carbon fiber, carbon nanotube, transparent colloid
Calcium is gentle/liquid phase silica in it is one or more.
Further, the carbon black preferable particle size is 0.01 ~ 100 μm, and conducting particles is spherical conductive particle, rod conductive
Particle and branched chain type conducting particles it is one or more.
The water-soluble resin is in waterborne polyurethane resin, acrylic resin aqueous solution and cellulosic resin
It is one or more.
The solvent is saturation halogen or class halogen solutions.It is preferred that solution is saturation halogen solutions, such as it is saturated bromine solutions, satisfies
And iodine solution.
The auxiliary agent be antifoaming agent, levelling agent, thickener, cohesive force accelerating agent and one kind in adhesion promoter or
It is a variety of；The antifoaming agent is organic silicon defoamer or polyether-type antifoaming agent；The levelling agent is organic silicon modified by polyether levelling agent
Or acrylic acid levelling agent；The thickener is cellulose thickener or inorganic thickening agent；The cohesive force accelerating agent is silane
Coupling agent or low molecular weight polyester resin；The adhesion promoter is to promote containing amino silane or adhesive force containing epoxy radicals silicone hydride
Agent.
The pH value of electrically conductive ink after step b) preparations is between 7.5 ~ 9.
Beneficial effects of the present invention：Graphene-based water-soluble conducting ink, solvent are saturation halogen solutions, are grinding initial mistake
Cheng Zhong, the halogenic molecule in solution can carry out intercalation between expanded graphite lamella, reduce the effect between expanded graphite lamella
Power and then increase Expandable graphite sheet layer number.At the same time, conductive filler can be filled between expanded graphite lamella, be formed three-dimensional
Conductive network structure further reduces the stacking between graphite flake and enhances the firmness between expanded graphite lamella.With
The growth of milling time, expanded graphite is gradually stripped into single-layer or multi-layer graphene so that whole ink electric conductivity is big
Width improves.
The graphene-based water-soluble conducting ink of the present invention, preparation method is simple, can be obtained using one step of high pressure homogenizer
Electrically conductive ink slurry, and it is not necessarily to abrasive media, save consumptive material, low-carbon environment-friendly.
Description of the drawings
Fig. 1 is that the TEM of 1 graphene-based water-soluble conducting ink of embodiment schemes.
Fig. 2 is silk-screen printing design sketch of the 1 graphene-based water-soluble conducting ink of embodiment in pet sheet face.
Fig. 3 is the relational graph of embodiment 1 graphene-based water-soluble conducting ink surface temperature and time.
Specific implementation mode
In order to further appreciate that the above-mentioned purpose and feature of the present invention, the present invention is explained in detail with reference to example
It states.
Provide a kind of graphene-based water-soluble conducting ink in the embodiment of the present invention, the preferred carbon black of the conducting particles, thoroughly
Gelatin matter calcium or and silica, binder be waterborne polyurethane resin, solvent is desaturation halogen solutions, and auxiliary agent is defoaming
Agent, levelling agent, thickener and adhesion promoter can be mixed with arbitrary proportion.
Embodiment 1
A kind of preparation method of modified graphite alkenyl water-soluble conducting ink, including 80 parts of bromine solutions of saturation are weighed respectively, expand stone
5 parts of ink, 4 parts of antifoaming agent, 1 part of levelling agent, 1 part of thickener, 1 part of adhesion promoter, 20 parts of superconduction carbon black, 25 parts of additions of resin
It is ground to the shearing of high pressure homogenizer mesohigh up to graphene-based water-soluble conducting ink.
Embodiment 2
80 parts of bromine solutions of saturation, 5 parts of expanded graphite, 6 parts of antifoaming agent, 3 parts of levelling agent, 1.5 parts of thickener, adhesive force are weighed respectively
1 part of accelerating agent, 10 parts of superconduction carbon black, 10 parts of aerosil, 30 parts of resin are added to the shearing of high pressure homogenizer mesohigh and grind
It grinds up to graphene-based water-soluble conducting ink.
Embodiment 3
80 parts of iodine solution of saturation, 6 parts of expanded graphite, 3 parts of antifoaming agent, 1 part of levelling agent, 2 parts of thickener, adhesive force are weighed respectively
1 part of accelerating agent, 10 parts of superconduction carbon black, 10 parts of liquid phase silica, 30 parts of resin are added to the shearing of high pressure homogenizer mesohigh and grind
It grinds up to graphene-based water-soluble conducting ink 3.
Embodiment 4
70 parts of iodine solution of saturation, 6 parts of expanded graphite, 3 parts of antifoaming agent, 1 part of levelling agent, 2 parts of thickener, adhesive force are weighed respectively
1 part of accelerating agent, 15 parts of carbon black, 10 parts of liquid phase silica, 40 parts of resin are added to high pressure homogenizer mesohigh shearing grinding i.e.
Obtain graphene-based water-soluble conducting ink.
Embodiment 5
70 parts of iodine solution of saturation, 8 parts of expanded graphite, 3 parts of antifoaming agent, 1 part of levelling agent, 2 parts of thickener, adhesive force are weighed respectively
1 part of accelerating agent, 1 part of cohesive force accelerating agent, 15 parts of carbon black, 15 parts of aerosil, 40 parts of resin are added to high pressure homogenizer
Mesohigh shearing is ground up to graphene-based water-soluble conducting ink.
Embodiment 6
70 parts of iodine solution of saturation, 8 parts of expanded graphite, 3 parts of antifoaming agent, 1 part of levelling agent, 2 parts of thickener, adhesive force are weighed respectively
1 part of accelerating agent, 1 part of cohesive force accelerating agent, 20 parts of carbon black, 15 parts of transparent calcium carbonate, 40 parts of resin are added in high pressure homogenizer
High shear grinds up to graphene-based water-soluble conducting ink.
Graphene-based water-soluble conducting ink prepared by above-mentioned each example, materialses and carries out testing graininess；Ink is taken to be coated with
In on transparent glass sheet or PET, 60 DEG C of solidification 15min carry out it resistivity and adhesive force test, as a result such as table 1
1 graphene-based water-soluble conducting ink performance test of table
By taking embodiment 1 as an example, by graphene-based water-soluble conducting ink, sampling carries out TEM tests, as shown in Figure 1, graphene sheet layer
It is relatively thin, it is substantially not present stacking phenomenon, and lamella size, between micron, sub-micron, distribution is relatively uniform；Pass through silk-screen printing
Mode be coated on PET, 120 DEG C of dry 30min, as shown in Fig. 2, resistivity in 0.05 Ω cm, then carry out electrical property and
Heating property is tested, as shown in figure 3, electrically conductive ink liter temperature rate is very fast, is brought rapidly up in 30s to 55 DEG C or so and heat generation
It can stablize, 55 DEG C are remained at after 50h.
It can be seen from Table 1 that graphene-based water-soluble conducting ink adhesive force prepared by one-step method is excellent, in glass and
0 grade is reached above PET；In addition, resistivity also has almost no change in different substrates, this has benefited from halogen point
The three-dimensional conductive network structure that son, conductive filler and expanded graphite lamella are formed, reduces the stacking between graphite flake, enhances
Firmness between expanded graphite lamella improves the electric conductivity of ink.
The foregoing is merely presently preferred embodiments of the present invention, the protection domain being not intended to limit the invention, every hair
Within bright spirit and principle, made by any modification or equivalent replacement, improvement etc., protection scope of the present invention should all be included in
Within.
Claims (9)
1. a kind of one-step method prepares graphene-based water-soluble conducting ink, which is characterized in that including following mass component：Expanded graphite
1 ~ 10 part of 1 ~ 8 part, 10 ~ 30 parts of conductive filler, 10 ~ 50 parts of water-soluble resin, 20 ~ 80 parts of solvent and auxiliary agent.
2. a kind of one-step method according to claim 1 prepares graphene-based water-soluble conducting ink, it is characterised in that：It is described to lead
The charged particle of electric filler include superconduction carbon black, acetylene black, carbon fiber, carbon nanotube, transparent calcium carbonate it is gentle/liquid phase silica
In it is one or more.
3. wanting a kind of one-step method described in 2 to prepare graphene-based water-soluble conducting ink according to right, it is characterised in that：Described leads
The conducting particles of electric filler is the one or more of spherical conductive particle, rod conductive particle and branched chain type conducting particles.
4. a kind of one-step method according to claim 1 prepares graphene-based water-soluble conducting ink, it is characterised in that：The water
Soluble resin is one or more in waterborne polyurethane resin, acrylic resin aqueous solution and cellulosic resin.
5. a kind of one-step method according to claim 1 prepares graphene-based water-soluble conducting ink, it is characterised in that：Described
Solvent is saturation halogen or class halogen solutions.
6. a kind of one-step method according to claim 1 prepares graphene-based water-soluble conducting ink, it is characterised in that：Described
Auxiliary agent is organic silicon defoamer, polyether-type antifoaming agent, organic silicon modified by polyether levelling agent, acrylic acid levelling agent, cellulose family increasing
Thick dose, inorganic thickening agent, silane coupling agent, low molecular weight polyester resin, containing amino silane or containing epoxy radicals silicone hydride attachment make every effort to promote
It is one or more into agent.
7. a kind of one-step method according to claim 1 prepares graphene-based water-soluble conducting ink, it is characterised in that：Described
The pH value of electrically conductive ink is between 7.5 ~ 9.
8. a kind of preparation method of graphene-based water-soluble conducting ink according to claim 1, specifically includes following steps,
It is characterized in that：
A) each component raw material is weighed by mass component ratio, wherein solvent weighs under the conditions of being protected from light；
B) under the conditions of being protected from light, solvent, expanded graphite, water-soluble resin, conductive filler and auxiliary agent are added to high pressure together
High shear grinding is carried out in homogenizer, you can obtain watersoluble plumbago alkene denatured conductive ink.
9. a kind of preparation method of graphene-based water-soluble conducting ink according to claim 8, it is characterised in that：Described
High pressure homogenizer is 207Mpa using pressure.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN109652014A (en) * | 2018-12-26 | 2019-04-19 | 宁波杉元石墨烯科技有限公司 | A kind of graphene dispersion grinding aid and preparation method thereof |
| CN109811380A (en) * | 2019-03-21 | 2019-05-28 | 华侨大学 | A kind of conducting surface treatment method before ABS plastic plating |
| CN109971256A (en) * | 2019-03-29 | 2019-07-05 | 兰州大学 | High-performance graphene electrically conductive ink and preparation method thereof is prepared in situ in a kind of one-step method |
| CN110467847A (en) * | 2019-08-21 | 2019-11-19 | 厦门大学 | A kind of preparation method of aqueous carbon series conductive ink and aqueous carbon series conductive ink |
| CN110628264A (en) * | 2019-08-21 | 2019-12-31 | 厦门大学 | Preparation method of graphene far-infrared additive and far-infrared slurry |
| CN111073396A (en) * | 2020-01-19 | 2020-04-28 | 浙江纳美新材料股份有限公司 | Graphene-based water-based conductive ink and preparation method thereof |
| CN111704830A (en) * | 2020-07-22 | 2020-09-25 | 广东一纳科技有限公司 | Graphene printing ink derived from expanded graphite and preparation method and application thereof |
| CN111875961A (en) * | 2020-08-12 | 2020-11-03 | 西北大学 | High-dispersion graphene composite material with short-chain polymer adsorbed on surface and preparation method thereof |
| WO2021031464A1 (en) * | 2019-08-21 | 2021-02-25 | 厦门大学 | Method for preparing graphene far infrared additive and far infrared paste |
| CN113122072A (en) * | 2019-12-30 | 2021-07-16 | 山东欧铂新材料有限公司 | Graphene conductive ink for heating film and preparation method thereof |
| CN113388270A (en) * | 2021-05-11 | 2021-09-14 | 宁波石墨烯创新中心有限公司 | Modified spherical carbon particle material, graphene-based water-based conductive ink containing same and preparation method of graphene-based water-based conductive ink |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652014A (en) * | 2018-12-26 | 2019-04-19 | 宁波杉元石墨烯科技有限公司 | A kind of graphene dispersion grinding aid and preparation method thereof |
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN109811380A (en) * | 2019-03-21 | 2019-05-28 | 华侨大学 | A kind of conducting surface treatment method before ABS plastic plating |
| CN109811380B (en) * | 2019-03-21 | 2022-06-10 | 华侨大学 | Conductive surface treatment method before electroplating of ABS (acrylonitrile butadiene styrene) plastic |
| CN109971256A (en) * | 2019-03-29 | 2019-07-05 | 兰州大学 | High-performance graphene electrically conductive ink and preparation method thereof is prepared in situ in a kind of one-step method |
| WO2021031464A1 (en) * | 2019-08-21 | 2021-02-25 | 厦门大学 | Method for preparing graphene far infrared additive and far infrared paste |
| CN110628264A (en) * | 2019-08-21 | 2019-12-31 | 厦门大学 | Preparation method of graphene far-infrared additive and far-infrared slurry |
| CN110467847A (en) * | 2019-08-21 | 2019-11-19 | 厦门大学 | A kind of preparation method of aqueous carbon series conductive ink and aqueous carbon series conductive ink |
| CN113122072A (en) * | 2019-12-30 | 2021-07-16 | 山东欧铂新材料有限公司 | Graphene conductive ink for heating film and preparation method thereof |
| CN111073396A (en) * | 2020-01-19 | 2020-04-28 | 浙江纳美新材料股份有限公司 | Graphene-based water-based conductive ink and preparation method thereof |
| CN111704830A (en) * | 2020-07-22 | 2020-09-25 | 广东一纳科技有限公司 | Graphene printing ink derived from expanded graphite and preparation method and application thereof |
| CN111875961A (en) * | 2020-08-12 | 2020-11-03 | 西北大学 | High-dispersion graphene composite material with short-chain polymer adsorbed on surface and preparation method thereof |
| CN111875961B (en) * | 2020-08-12 | 2021-05-07 | 西北大学 | High-dispersion graphene composite material with short-chain polymer adsorbed on surface and preparation method thereof |
| CN113388270A (en) * | 2021-05-11 | 2021-09-14 | 宁波石墨烯创新中心有限公司 | Modified spherical carbon particle material, graphene-based water-based conductive ink containing same and preparation method of graphene-based water-based conductive ink |
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Application publication date: 20180914 |