CN111808477A - Water-based graphene conductive ink and preparation method thereof - Google Patents
Water-based graphene conductive ink and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 44
- 239000010439 graphite Substances 0.000 claims abstract description 44
- 239000002952 polymeric resin Substances 0.000 claims abstract description 29
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 29
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- -1 aldehyde ketone Chemical class 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000003085 diluting agent Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 229920000180 alkyd Polymers 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 239000002318 adhesion promoter Substances 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 239000003899 bactericide agent Substances 0.000 claims description 2
- QHIWVLPBUQWDMQ-UHFFFAOYSA-N butyl prop-2-enoate;methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C.CCCCOC(=O)C=C QHIWVLPBUQWDMQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- MTSKWRIATJSKFJ-XPOVZDRTSA-N glucosone Chemical compound OCC(O)[C@H]1O[C@@H](O)C(=O)[C@@H]1O MTSKWRIATJSKFJ-XPOVZDRTSA-N 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920001225 polyester resin Polymers 0.000 claims description 2
- 239000004645 polyester resin Substances 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- 239000013008 thixotropic agent Substances 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 9
- 238000007639 printing Methods 0.000 abstract description 9
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000012776 electronic material Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 description 4
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000007641 inkjet printing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000009450 smart packaging Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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
-
- 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
- C09D11/023—Emulsion inks
- C09D11/0235—Duplicating inks, e.g. for stencil printing
-
- 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
- C09D11/10—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
- C09D11/103—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds of aldehydes, e.g. phenol-formaldehyde resins
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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
- C09D11/105—Alkyd resins
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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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Conductive Materials (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The embodiment of the invention discloses water-based graphene conductive ink and a preparation method thereof, and belongs to the technical field of printed electronic materials. The water-based graphene conductive ink is prepared from the following raw materials in percentage by weight: 0.1-30% of expandable graphite, 0.5-15.4% of water-based polymer resin, 0.1-30% of auxiliary agent and 30-97.4% of solvent. The aqueous graphene of the invention is conductiveThe ink has remarkable advantage in conductive performance, and the conductivity can reach 1.87 multiplied by 104‑3.79×104S/m, and has the advantages of light weight of printed patterns, good printing adaptability, mild curing conditions, low cost and the like. Meanwhile, the raw materials are low in price, harmless and nontoxic to human bodies and the environment, meet the requirements of ecological friendliness and sustainable development, and meet the requirement of industrial production.
Description
Technical Field
The embodiment of the invention relates to the technical field of printed electronic materials, and particularly relates to aqueous graphene conductive ink and a preparation method thereof.
Background
Printed electronics are electronic devices and circuits made by printing techniques, which are moving toward flexibility, low cost, and high performance. The traditional preparation processes of electronic devices mainly comprise photoetching, vacuum deposition and chemical plating, and the methods have the disadvantages of multiple steps, high equipment cost and environmental pollution.
In recent years, with the development of material science and technology, new electronic printing technology is also 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.
Compared with the traditional printing electronic process, the conductive ink printing electronic process has the advantages of simple and direct production process, low-temperature operation, small raw material loss, small equipment investment, flexibility and large-area production, more importantly, can eliminate the environmental protection problems of waste liquid discharge and the like caused by the traditional printing process, and is an environment-friendly manufacturing technology.
With the rapid development of the 21 st century nanotechnology, the nanoscale conductive ink attracts great attention at home and abroad by virtue of the high-speed industrialization of the printed electronic technology, and the application of the nanoscale conductive ink in the fields of radio frequency identification systems, intelligent packaging, printed circuit boards and the like is increasing day by day. At present, the nano metal conductive ink is applied to the field of flexible electronics such as conductive electrodes, optoelectronic devices, radio frequency identification and biosensors, and compared with the nano metal conductive ink, the graphene conductive ink has the advantages of outstanding cost, better conductivity and compatibility with an ink-jet printing mode compared with the traditional carbon conductive ink.
Disclosure of Invention
Therefore, the embodiment of the invention provides water-based graphene conductive ink and a preparation method thereof.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
according to a first aspect of the embodiments of the present invention, an embodiment of the present invention provides an aqueous graphene conductive ink, which is prepared from the following raw materials in percentage by weight: 0.1-30% of expandable graphite, 0.5-15.4% of water-based polymer resin, 0.1-30% of auxiliary agent and 30-97.4% of solvent.
Further, the aqueous graphene conductive ink is prepared from the following raw materials in percentage by weight: 5-15% of expandable graphite, 2-13% of water-based polymer resin, 0.1-5% of auxiliary agent and 35-85% of solvent.
Further, the number of layers of expandable graphite is less than 300.
Further, the aqueous polymer resin is selected from one or more of cellulose derivatives, aldehyde ketone resins, alkyd resins, polyester resins, phenolic resins, acrylic resins and polyacrylates.
Further, the auxiliary agent is selected from one or more of an adhesion promoter, a reactive diluent, a thickening agent, a plasticizer, a thixotropic agent, a stabilizer, a bactericide, a wetting dispersant, a coupling agent, an accelerator, a leveling agent, an antifoaming agent and a film-forming auxiliary agent.
Further, the solvent is selected from one or more of deionized water, ethanol, butanol, isopropanol and dihydrovinyl glucosone.
According to a second aspect of the embodiments of the present invention, there is provided a method for preparing the above aqueous graphene conductive ink, the method including the following steps:
(1) heating the ceramic crucible containing the expandable graphite in a microwave oven, washing with deionized water to remove residual acid liquor in the raw materials, and drying at 90-110 ℃ for 4-6h to obtain worm-shaped graphite with volume expansion of 4-6 times;
(2) putting the aqueous polymer resin, the auxiliary agent and the solvent into a dispersion kettle, stirring to completely swell and dissolve the aqueous polymer resin, and obtaining aqueous polymer resin slurry with the viscosity of 5000-;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) and transferring the graphite coarse slurry to a three-roll grinder to grind until the particle size is less than 1 mu m, thus obtaining the aqueous graphene conductive ink.
In the step (2), when the viscosity of the aqueous polymer resin slurry is 5000-.
Further, in the step (1), the power of the microwave oven is 600- & lt 1000 & gt W, and the heating time is 10-60 s.
Further, in the step (4), the roller gap of the three-roller grinding machine is 1 μm, and the rotation speed ratio of the three rollers is 1: 3: 9.
the aqueous graphene conductive ink prepared by the invention has excellent conductive performance, can be used for manufacturing thin film switches, transparent conductive films, touch screens, liquid crystal displays, plasma displays, Printed Circuit Boards (PCBs), flexible circuit boards and circuit boards, thin film keyboards, electromagnetic shields, flexible conductive flat cables, bendable flexible electronic products, chemical and biological sensors, electronic skins, lithium ion batteries, printed batteries, solar photovoltaic batteries, Electroluminescent (EL) light sources, Organic Light Emitting Diodes (OLEDs), display devices and equipment, radio frequency identification tags (RFID) and other products and next-generation light, thin and flexible electronic products, and has wide market prospect.
The raw materials used in the invention are introduced as follows:
the aqueous polymer resin is used as a film forming substance in the conductive ink, plays a role of a bridge skeleton, and can enable graphene sheets to be uniformly dispersed to form a three-dimensional conductive network.
And the auxiliary agents are commonly used in the field of ink, and can improve the conductivity, stability, surface performance of printed products, printing adaptability and the like of the ink.
The solvent has the functions of dissolving the resin and the auxiliary agent, improving the printing adaptability of the ink and adjusting the viscosity and the drying speed.
The embodiment of the invention has the following advantages:
1. the aqueous graphene conductive ink is prepared from expandable graphite, aqueous polymer resin, an auxiliary agent and a solvent, wherein the expandable graphite is subjected to microwave heating and three-roller grinding treatment to generate the graphene with a honeycomb two-dimensional carbon lattice. Compared with the traditional carbon-based conductive ink product, the aqueous graphene conductive ink prepared by the invention has remarkable advantage in conductivity, and the conductivity can reach 1.87 multiplied by 104-3.79×104S/m, and has the advantages of light weight of printed patterns, good printing adaptability, mild curing condition, low cost and the like.
2. The water-based polymer resin, the auxiliary agent and the solvent used in the invention have low prices, are harmless and nontoxic to human bodies and environment, meet the requirements of ecological friendliness and sustainable development, and meet the requirement of industrial production.
3. The graphene is adopted to replace metal fillers such as silver powder, copper powder and the like, so that the filling amount of the conductive fillers is reduced, the density of the ink and the coating is reduced, and the graphene conductive ink has the advantages of sedimentation resistance, low cost, no heavy metal pollution, easiness in recovery and the like. And the traditional expensive and time-consuming etching technology is replaced, so that the waste of metal materials is reduced.
4. The three-roller grinding process can enable the particle size distribution of the slurry to be more uniform and concentrated, is convenient for ink jet or screen printing, has simple production process and low cost consumption, is suitable for large-scale industrial production, and simultaneously enables graphene sheets randomly stacked in a bonding base material to be arranged in a layered manner to enhance the conductivity.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the aqueous graphene conductive ink comprises the following steps:
(1) placing a ceramic crucible containing 100g of expandable graphite in a microwave oven with the power of 800W, heating for 30s, washing with deionized water to remove acid liquor remained in the raw materials, and drying at 100 ℃ for 5h to obtain worm-shaped graphite with the volume expanded by 5 times;
(2) putting 56g of aqueous aldehyde ketone resin, 4g of 2-amino-2-methyl-1-propanol, 200g of ethanol and 640g of deionized water into a dispersion kettle, and stirring to completely swell and dissolve the mixture to obtain aqueous polymer resin slurry with the viscosity of 7000 Pa.s;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) transferring the graphite coarse slurry into a three-roll grinder to be fully ground until the particle size is less than 1 mu m, wherein the roll gap of the used three-roll grinder is 1 mu m, and the rotation speed ratio of three rolls is 1: 3: and 9, preparing the water-based graphene conductive ink.
After the ink was coated and dried, the resistivity of the aqueous graphene conductive ink was measured to be 0.0053 Ω · cm, i.e., the conductivity was 1.87 × 10, using a four-probe4S/m。
Example 2
The preparation method of the aqueous graphene conductive ink comprises the following steps:
(1) placing a ceramic crucible containing 100g of expandable graphite in a microwave oven with power of 600W, heating for 60s, washing with deionized water to remove acid liquor remained in the raw materials, and drying at 90 ℃ for 6h to obtain worm-shaped graphite with volume expansion of 5.5 times;
(2) putting 60g of alkyd resin, 4g of reactive diluent, 236g of ethanol and 600g of deionized water into a dispersion kettle, and stirring to completely swell and dissolve the alkyd resin to obtain aqueous polymer resin slurry with viscosity of 20000 Pa.s;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) transferring the graphite coarse slurry into a three-roll grinder to be fully ground until the particle size is less than 1 mu m, wherein the roll gap of the used three-roll grinder is 1 mu m, and the rotation speed ratio of three rolls is 1: 3: and 9, preparing the water-based graphene conductive ink.
After the ink is coated and dried, the resistivity of the aqueous graphene conductive ink is measured to be 0.0026 omega cm by using a four-probe, namely the conductivity is 3.97 multiplied by 104S/m。
Example 3
The preparation method of the aqueous graphene conductive ink comprises the following steps:
(1) placing a ceramic crucible containing 100g of expandable graphite in a microwave oven with the power of 1000W, heating for 20s, washing with deionized water to remove acid liquor remained in the raw materials, and drying at 110 ℃ for 4h to obtain worm-shaped graphite with the volume expanded by 4.8 times;
(2) putting 60g of phenolic resin, 4g of active diluent, 136g of butanol and 700g of deionized water into a dispersion kettle, and stirring to completely swell and dissolve the phenolic resin, the active diluent and the butanol to obtain aqueous polymer resin slurry with the viscosity of 12000 Pa.s;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) transferring the graphite coarse slurry into a three-roll grinder to be fully ground until the particle size is less than 1 mu m, wherein the roll gap of the used three-roll grinder is 1 mu m, and the rotation speed ratio of three rolls is 1: 3: and 9, preparing the water-based graphene conductive ink.
After the ink is coated and dried, the resistivity of the aqueous graphene conductive ink is measured to be 0.0046 omega cm by using a four-probe, namely the conductivity is 2.17 multiplied by 104S/m。
Comparative example 1
The preparation method of the aqueous graphene conductive ink of the comparative example includes the following steps:
(1) placing a ceramic crucible containing 100g of expandable graphite in a microwave oven with the power of 800W, heating for 30s, washing with deionized water to remove acid liquor remained in the raw materials, and drying at 100 ℃ for 5h to obtain worm-shaped graphite with the volume expanded by 5 times;
(2) putting 200g of water-based aldehyde ketone resin, 4g of 2-amino-2-methyl-1-propanol, 200g of ethanol and 640g of deionized water into a dispersion kettle, and stirring to completely swell and dissolve the water-based aldehyde ketone resin, the ethanol and the deionized water to obtain water-based polymer resin slurry with the viscosity of 40000 Pa.s;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) transferring the graphite coarse slurry into a three-roll grinder to be fully ground until the particle size is less than 1 mu m, wherein the roll gap of the used three-roll grinder is 1 mu m, and the rotation speed ratio of three rolls is 1: 3: and 9, preparing the water-based graphene conductive ink.
The resistivity of the aqueous graphene conductive ink is 63 omega cm, namely the conductivity is 1.59S/m.
Comparative example 2
The preparation method of the aqueous graphene conductive ink of the comparative example includes the following steps:
(1) placing a ceramic crucible containing 100g of expandable graphite in a microwave oven with the power of 800W, heating for 30s, washing with deionized water to remove acid liquor remained in the raw materials, and drying at 100 ℃ for 5h to obtain worm-shaped graphite with the volume expanded by 5 times;
(2) putting 20g of aqueous aldehyde ketone resin, 4g of 2-amino-2-methyl-1-propanol, 200g of ethanol and 640g of deionized water into a dispersion kettle, and stirring to completely swell and dissolve the aqueous aldehyde ketone resin, the 4g of 2-amino-2-methyl-1-propanol to obtain aqueous polymer resin slurry with the viscosity of 2000 Pa.s;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) transferring the graphite coarse slurry into a three-roll grinder to be fully ground until the particle size is less than 1 mu m, wherein the roll gap of the used three-roll grinder is 1 mu m, and the rotation speed ratio of three rolls is 1: 3: and 9, preparing the water-based graphene conductive ink.
The resistivity of the aqueous graphene conductive ink is 0.79 omega cm, namely the conductivity is 1.27 multiplied by 102S/m。
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The water-based graphene conductive ink is characterized by being prepared from the following raw materials in percentage by weight: 0.1-30% of expandable graphite, 0.5-15.4% of water-based polymer resin, 0.1-30% of auxiliary agent and 30-97.4% of solvent.
2. The aqueous graphene conductive ink according to claim 1, wherein the aqueous graphene conductive ink is prepared from the following raw materials in percentage by weight: 5-15% of expandable graphite, 2-13% of water-based polymer resin, 0.1-5% of auxiliary agent and 35-85% of solvent.
3. The aqueous graphene conductive ink according to claim 1, wherein the number of layers of expandable graphite is less than 300.
4. The aqueous graphene conductive ink according to claim 1, wherein the aqueous polymer resin is selected from one or more of cellulose derivatives, aldehyde ketone resins, alkyd resins, polyester resins, phenolic resins, acrylic resins, and polyacrylates.
5. The aqueous graphene conductive ink according to claim 1, wherein the auxiliary agent is one or more selected from an adhesion promoter, a reactive diluent, a thickener, a plasticizer, a thixotropic agent, a stabilizer, a bactericide, a wetting dispersant, a coupling agent, an accelerator, a leveling agent, an antifoaming agent, and a film-forming auxiliary agent.
6. The aqueous graphene conductive ink according to claim 1, wherein the solvent is one or more selected from deionized water, ethanol, butanol, isopropanol, and dihydrovinyl glucosone.
7. A preparation method of the aqueous graphene conductive ink according to claim 1, wherein the method comprises the following steps:
(1) heating the ceramic crucible containing the expandable graphite in a microwave oven, washing with deionized water to remove residual acid liquor in the raw materials, and drying at 90-110 ℃ for 4-6h to obtain worm-shaped graphite with volume expansion of 4-6 times;
(2) putting the aqueous polymer resin, the auxiliary agent and the solvent into a dispersion kettle, stirring to completely swell and dissolve the aqueous polymer resin, and obtaining aqueous polymer resin slurry with the viscosity of 5000-;
(3) mixing the vermicular graphite prepared in the step (1) and the aqueous polymer resin slurry prepared in the step (2), and uniformly stirring to obtain graphite coarse slurry;
(4) and transferring the graphite coarse slurry to a three-roll grinder to grind until the particle size is less than 1 mu m, thus obtaining the aqueous graphene conductive ink.
8. The method for preparing the aqueous graphene conductive ink as claimed in claim 7, wherein in the step (1), the power of the microwave oven is 600-1000W, and the heating time is 10-60 s.
9. The preparation method of the aqueous graphene conductive ink according to claim 7, wherein in the step (4), the roller gap of the three-roller mill is 1 μm, and the rotation speed ratio of the three rollers is 1: 3: 9.
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Application publication date: 20201023 |