CN111793389A - Preparation process of graphene conductive slurry - Google Patents
Preparation process of graphene conductive slurry Download PDFInfo
- Publication number
- CN111793389A CN111793389A CN202010693744.1A CN202010693744A CN111793389A CN 111793389 A CN111793389 A CN 111793389A CN 202010693744 A CN202010693744 A CN 202010693744A CN 111793389 A CN111793389 A CN 111793389A
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- Prior art keywords
- conductive paste
- graphene
- graphene conductive
- ink
- paste
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Classifications
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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
- C09D11/30—Inkjet printing 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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention relates to the field of conductive paste, in particular to a preparation process of graphene conductive paste, which comprises the following steps: 1) pretreatment of graphite: pretreating flake graphite by using a mixture composed of potassium permanganate and concentrated sulfuric acid according to a certain proportion; 2) stripping: adding a reagent into the oxidation product, mixing DMF and water in a certain volume ratio to serve as a solvent, and ultrasonically stripping; 3) and (3) replacement: adding a mixed solvent of cyclohexanone and terpineol for replacement; 4) and adding an auxiliary agent, dispersing and filtering to obtain the graphene conductive slurry. The ink with good dispersion can be prepared by mixing DMF and water as a solvent, and the stripping of graphite flakes can be enhanced by mixing the polyvinyl alcohol and the graphite oxide, so that stable ink-jet printing can be provided. The ethyl cellulose is used as a stabilizer, the viscosity and the surface tension of the conductive paste are adjusted by adopting ethanol to meet the requirements of ink-jet printing, the prepared graphene ink is high in concentration and good in stability, and the fluid characteristics of the graphene ink meet the technical requirements of ink-jet printing.
Description
Technical Field
The invention belongs to the field of conductive paste, and particularly relates to a preparation process of graphene conductive paste.
Background
In recent years, with the development of material science and technology, new electronic printing technology is continuously advanced, the substrate of the flexible printed circuit is not limited to plastic substrate, and paper, textile, silicon rubber and ultra-thin glass can be used for manufacturing flexible electronic devices and coating circuits. Therefore, the market needs conductive paste with higher conductivity, and graphene and composite graphene material conductive paste are greatly concerned.
Compared with the traditional printing electronic process, the conductive paste printing electronic process has the advantages of simple and direct production process, small raw material loss, less equipment investment, flexibility and capability of realizing large-area production, and more importantly, the conductive paste printing electronic process can eliminate the environmental protection problems of waste liquid discharge and the like caused by the traditional printing process, thereby being an environment-friendly manufacturing technology.
The conductive paste is mainly divided into metal conductive paste, carbon conductive paste and the like, and the conductive paste of silver nano material is most used in the market at present, but the raw material price is too expensive; although the raw materials of the copper-based conductive paste are relatively cheap, the application of the copper-based conductive paste is limited to a certain extent due to the easily-oxidized property.
The resistivity of the carbon-based ink sold in the market at present is generally higher, the conductive effect is not ideal, and graphene is easy to agglomerate. The high-performance screen printing ink prepared by utilizing the graphene is expected to obtain the same conductivity as the silver conductive paste, better usability and stability, and meanwhile, the ink cost is reduced, so that the development of a flexible printing electronic technology is promoted.
Disclosure of Invention
The invention aims to provide a preparation process of graphene conductive paste, and aims to solve the problem that the conductivity of the existing graphene conductive paste cannot be effectively improved due to the fact that graphene is easy to agglomerate.
The invention adopts the following technical scheme:
the preparation process of the graphene conductive paste comprises the following steps:
1) pretreatment of graphite
Pretreating and oxidizing the flake graphite by utilizing a mixture composed of potassium permanganate and concentrated sulfuric acid according to a certain proportion;
2) peeling off
Adding a reagent into the oxidation product obtained in the step 1), mixing DMF and water in a certain volume ratio to serve as a solvent, and ultrasonically stripping;
3) replacement of
Adding a mixed solvent of cyclohexanone and terpineol for replacement;
4) adding an auxiliary agent
And adding an auxiliary agent, dispersing and filtering to obtain the graphene conductive slurry.
Preferably, in the step 1), the weight ratio of potassium permanganate to concentrated sulfuric acid is 14-20: 1;
the weight ratio of the crystalline flake graphite to the potassium perchlorate powder is 100-150: 1;
the weight part of the concentrated sulfuric acid is 95-98 wt.%.
Preferably, in the step 1), the pretreatment time of the crystalline flake graphite by potassium permanganate and concentrated sulfuric acid is 35-45min, and the pretreatment temperature is 52-58 ℃.
Preferably, in the step 2), the volume ratio of DMF to water is 10-13: 1.
preferably, in step 2), the reagent used for stripping is polyvinyl alcohol.
Preferably, in step 3), the weight ratio of cyclohexanone to terpineol is 80-84: 16.
Preferably, in step 4), the auxiliary agent comprises one or more of a stabilizer, a linking agent, a surfactant and a regulator.
Preferably, the stabilizer in the auxiliary agent is ethyl cellulose and/or ethanol.
Preferably, the connecting agent in the auxiliary agent is an E-51 type epoxy resin and/or an E-44 type epoxy resin.
Compared with the prior art, the invention has the following beneficial effects:
the ink with good dispersion can be prepared by mixing DMF and water as a solvent, and the stripping of graphite flakes can be enhanced by mixing the polyvinyl alcohol and the graphite oxide, so that stable ink-jet printing can be provided. The ethyl cellulose is used as a stabilizer, the viscosity and the surface tension of the conductive paste are adjusted by adopting ethanol to meet the requirements of ink-jet printing, the prepared graphene ink is high in concentration and good in stability, and the fluid characteristics of the graphene ink meet the technical requirements of ink-jet printing.
Detailed Description
Example 1
1) Pretreatment of graphite
Pretreating and oxidizing 100g of flake graphite at 52 ℃ for 35min by using a mixture consisting of 14g of potassium permanganate and 1g of concentrated sulfuric acid with the weight part being 95 wt.%;
2) peeling off
Adding a reagent into the oxidation product obtained in the step 1), mixing 13g of DMF (dimethyl formamide) and 1g of water as a solvent, and ultrasonically stripping;
3) replacement of
Adding a mixed solvent of 80g of cyclohexanone and 16g of terpineol for replacement;
4) adding an auxiliary agent
And sequentially adding 2g of ethanol and 5g of E-44 type epoxy resin as an auxiliary agent, and dispersing and filtering to obtain the graphene conductive slurry.
Example 2
1) Pretreatment of graphite
Pretreating 150g of flake graphite at 58 ℃ for oxidizing for 45min by using a mixture consisting of 20g of potassium permanganate and 1g of concentrated sulfuric acid with the weight part being 95 wt.%;
2) peeling off
Adding a reagent into the oxidation product obtained in the step 1), mixing 10g of DMF (dimethyl formamide) and 1g of water as a solvent, and ultrasonically stripping;
3) replacement of
Adding a mixed solvent of 84g of cyclohexanone and 16g of terpineol for replacement;
4) adding an auxiliary agent
And sequentially adding 2g of ethyl cellulose and 5g of E-51 type epoxy resin as an auxiliary agent, and dispersing and filtering to obtain the graphene conductive slurry.
Example 3
1) Pretreatment of graphite
Pretreating and oxidizing 100g of flake graphite for 40min at 55 ℃ by using a mixture consisting of 14g of potassium permanganate and 1g of concentrated sulfuric acid with the weight part being 95 wt.%;
2) peeling off
Adding a reagent into the oxidation product obtained in the step 1), mixing 11g of DMF (dimethyl formamide) and 1g of water as a solvent, and ultrasonically stripping;
3) replacement of
Adding a mixed solvent of 82g of cyclohexanone and 16g of terpineol for replacement;
4) adding an auxiliary agent
And 3g of ethanol and 5g E-44 type epoxy resin are sequentially added to serve as an auxiliary agent, and the graphene conductive slurry is obtained through dispersion and filtration.
Claims (9)
1. A preparation process of graphene conductive paste is characterized by comprising the following steps:
1) pretreatment of graphite
Pretreating and oxidizing the flake graphite by utilizing a mixture composed of potassium permanganate and concentrated sulfuric acid according to a certain proportion;
2) peeling off
Adding a reagent into the oxidation product obtained in the step 1), mixing DMF and water in a certain volume ratio to serve as a solvent, and ultrasonically stripping;
3) replacement of
Adding a mixed solvent of cyclohexanone and terpineol for replacement;
4) adding an auxiliary agent
And adding an auxiliary agent, dispersing and filtering to obtain the graphene conductive slurry.
2. The graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 1), the weight ratio of potassium permanganate to concentrated sulfuric acid is 14-20: 1;
the weight ratio of the crystalline flake graphite to the potassium permanganate powder is 100-150: 1;
the weight part of the concentrated sulfuric acid is 95-98 wt.%.
3. The graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 1), the pretreatment time of potassium permanganate and concentrated sulfuric acid on the crystalline flake graphite is 35-45min, and the pretreatment temperature is 52-58 ℃.
4. The graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 2), the volume ratio of DMF to water is 10-13: 1.
5. the graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 2), the reagent used for stripping is polyvinyl alcohol.
6. The graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 3), the weight ratio of the cyclohexanone to the terpineol is 80-84: 16.
7. The graphene conductive paste according to claim 1, wherein the conductive paste is a paste,
in the step 4), the auxiliary agent comprises one or more of a stabilizing agent, a connecting agent, a surfactant and a regulator.
8. The graphene conductive paste according to claim 7, wherein the conductive paste,
the stabilizer in the auxiliary agent is ethyl cellulose and/or ethanol.
9. The graphene conductive paste according to claim 7, wherein the conductive paste,
the connecting agent in the auxiliary agent is E-51 type epoxy resin and/or E-44 type epoxy resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010693744.1A CN111793389A (en) | 2020-07-17 | 2020-07-17 | Preparation process of graphene conductive slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010693744.1A CN111793389A (en) | 2020-07-17 | 2020-07-17 | Preparation process of graphene conductive slurry |
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| Publication Number | Publication Date |
|---|---|
| CN111793389A true CN111793389A (en) | 2020-10-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN202010693744.1A Pending CN111793389A (en) | 2020-07-17 | 2020-07-17 | Preparation process of graphene conductive slurry |
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| CN (1) | CN111793389A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882796A (en) * | 2017-03-23 | 2017-06-23 | 复旦大学 | A kind of preparation method of three-dimensional grapheme structure/high-quality graphene |
-
2020
- 2020-07-17 CN CN202010693744.1A patent/CN111793389A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882796A (en) * | 2017-03-23 | 2017-06-23 | 复旦大学 | A kind of preparation method of three-dimensional grapheme structure/high-quality graphene |
Non-Patent Citations (1)
| Title |
|---|
| 石小梅等: "石墨烯导电油墨的研究进展", 《包装工程》 * |
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Application publication date: 20201020 |