CN106167654A - A kind of copper conductive ink containing graphene oxide and its preparation method and application - Google Patents
A kind of copper conductive ink containing graphene oxide and its preparation method and application Download PDFInfo
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- CN106167654A CN106167654A CN201610475270.7A CN201610475270A CN106167654A CN 106167654 A CN106167654 A CN 106167654A CN 201610475270 A CN201610475270 A CN 201610475270A CN 106167654 A CN106167654 A CN 106167654A
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- copper
- conductive ink
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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
- C09D11/30—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)
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- Wood Science & Technology (AREA)
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Abstract
The invention discloses a kind of copper conductive ink containing graphene oxide and its preparation method and application, copper conductive ink percentage composition by weight, the component including following: graphene oxide, the copper powder of 0.5 90%, the resin of 1 50%, the wetting agent of 0 1%, the thixotropic agent of 0 1%, 0.5 1% thickening agent, the coupling agent of 0 1% and the solvent of 2 60% of 0.5 90%.The resistivity of described copper conductive ink is low, good stability, can be with long-term existence, will not be oxidized.
Description
Technical field
The present invention relates to a kind of copper conductive ink containing graphene oxide and its preparation method and application.
Background technology
Conductive ink is the basis of development electronic devices and components, is encapsulation, electrode and the critical material of interconnection, be collection metallurgical,
Chemical industry, electronic technology are in a kind of high-tech electronics functional material of one, mainly for the manufacture of thick film integrated circuit, sensitive unit
The every field of the electron trades such as part, capacitor, potentiometer, thick film hybrid integrated circuit, surface installation technique.In conductive ink
Conductive filler be typically made up of noble metal Au, Ag or base metal Cu, Ni, Al etc..The general good conductivity of noble metal, is difficult to oxygen
Change, if but use noble metal in a large number, production cost rises；And base metal is easier oxidation, after burning, impact is led
The electric conductivity of electricity ink.Additionally the sintering of base metal slurry is typically carried out under nitrogen or vacuum condition, and this technique can make
Cost increases, and operating process simultaneously is complicated.
At the beginning of the seventies, du pont company successfully develops the copper electrocondution slurry of the slug type under nitrogen protection, and in big face
Apply on long-pending ceramic substrate.Sintering process is required strict by this copper slurry, and the oxygen content of nitrogen have to be lower than 6 × 10-6, therefore become
This is almost consistent with the cost using conductive noble metal slurry.Can have at the copper conductive ink of atmospheric atmosphere sintering to develop
Researcher is by preparing copper silver, the copper alloy of copper nickel core-shell structure or boron-doping in main body base metal, silicon and other is golden
Belong to protective agent.And after material oxidation such as these protective agents such as boron and silicon etc., owing to its oxide is non-conductive or poorly conductive, finally
The electric conductivity of slurry will be affected.
Summary of the invention
It is an object of the invention to provide a kind of copper conductive ink containing graphene oxide steady in a long-term and preparation method
And application.By using graphene oxide, copper powder and other interpolation auxiliary agent to prepare conductive ink, wherein, copper powder and oxidation stone
Ink alkene can well disperse, and in dispersive process, a small amount of copper can be with the hydroxy-acid group reaction of graphene oxide so that copper is with ion shape
Formula forms graphene oxide copper carboxylate with the carboxylic acid of graphene oxide, and the most most copper and graphene oxide are dispersed.
This conductive ink can pass through printing, dip-coating, some glue and be sprayed in paper, glass, pottery and plastics and other base, at 250 DEG C
Below after sintering, graphene oxide can be reduced, and the graphene oxide copper carboxylate simultaneously formed in dispersive process can resolve into copper；
It addition, graphene oxide is due to the substantial amounts of oh group of content, in roasting process, it is possible to prevent copper to aoxidize further.The method
The conducting wire made, during life-time service, owing to Graphene is attached to copper surface so that copper is not oxidized, can be long-term
Stable existence.
In order to achieve the above object, the present invention provides a kind of copper conductive ink containing graphene oxide steady in a long-term, institute
State conductive ink and contain 0.5-90%(such as 30%, 50%, 70%) graphene oxide, 0.5-90%(such as 5%, 51%, 67%)
Copper powder, 1-50%(such as 10%, 30%, 40%) resin, the wetting agent of 0-1%, the thixotropic agent of 0-1%, 0.5-1% thickening agent, 0-1%
Coupling agent and the solvent of 2-60%.
Preferably, described graphene oxide accounts for the 30-50% of copper conductive ink weight, and the mass percent of each component it
With for 100%.Preferably, described copper powder accounts for the 30-70% of copper conductive ink weight, and the mass percent sum of each component is
100%。
Described graphene oxide is the oxidation stone of hydroxylating Graphene, carboxylated Graphene, different proportion hydroxycarboxyl group
Ink alkene or one or more of commercially available common graphene oxide.Contain the graphite oxide of hydroxyl and carboxyl the most simultaneously
Alkene；The more preferably mol ratio of hydroxyl and carboxyl is 1:3-3:1.
Described copper powder is spherical, the flake copper of a size of 1nm-20 μm, diameter 1nm-20 μm, the wire of length 1-50 μm
One or more in copper powder.
Described resin is binary vinyl chloride-vinyl acetate resin, ternary chlorine vinegar resin, Hydroxylated acrylic resin, mixed type hydroxyl polyester tree
One or many in fat, acrylic type polyester resin, ethyl cellulose, arabic gum, bisphenol-A epoxy and bisphenol F epoxy resin
Kind.
Described wetting agent is copolymer in cinnamic acrylic ester, polymine, the one of arabinogalactan or many
Kind.
Described thixotropic agent is polyamide wax, silicon dioxide, organobentonite, one or more of castor oil hydrogenated.
Described thickening agent is polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, arabic gum, methylcellulose
One or more.
Described solvent is water, ethanol, ethyl acetate, ethylene glycol, terpineol, tributyl citrate, nylon acid dimethyl ester
(DBE), one or more in DEGMBE.
The preparation method of described copper conductive ink comprises the steps of by weight percent, first by the resin of 1-50%,
The stirring solvent of the wetting agent of 0-1%, the thixotropic agent of 0-1%, 0.5-1% thickening agent, the coupling agent of 0-1% and 2-60% is uniform, very
Deaeration in empty agitator；The copper powder of the graphene oxide of 0.5-90%, 0.5-90% is successively added the mixture through deaeration
In, ultrasonic disperse；Then, being ground by the mixture after ultrasonic disperse, discharging is copper conductive ink.At 0 DEG C～8 DEG C after discharging
Cryogenic conditions under store.
During described ultrasonic disperse, copper powder and graphene oxide can well disperse, in dispersive process, a small amount of copper can and
The hydroxy-acid group reaction of graphene oxide so that copper forms graphite oxide olefinic carboxylic acid with the carboxylic acid of graphene oxide in the form of an ion
Copper, the most most copper and graphene oxide are dispersed.
Below 250 DEG C after sintering, graphene oxide can be reduced, the graphene oxide carboxylic simultaneously formed in dispersive process
Acid copper can resolve into copper；It addition, graphene oxide is due to the substantial amounts of oh group of content, in roasting process, it is possible to prevent copper to enter
Oxidation step.This sintering process can be carried out in atmospheric conditions.
Copper conductive ink passes through ink jet printing, aerosol injection printing, silk screen printing, intaglio printing, flexible printing, leaching
Be coated with, put glue and be sprayed in paper, glass, pottery, plastics and other base after, can be used for make RFID antenna, can wear
The interconnecting leads such as wearing electronic product, printed circuit board, flexible transparent electrode.
The conducting wire that the method makes, during life-time service, owing to Graphene is attached to copper surface so that copper is not
Oxidized, can exist steadily in the long term, keep good electric conductivity.
A kind of antioxidative of the present invention copper conductive ink containing graphene oxide and preparation method thereof, has following
Advantage:
1. in conductive ink roasting process, graphene oxide can be reduced, the graphene oxide carboxylic simultaneously formed in dispersive process
Acid copper can resolve into copper；
2., in roasting process, graphene oxide, due to the substantial amounts of oh group of content, is possible to prevent copper to aoxidize further；
3. the conducting wire that the method makes, during life-time service, Graphene is attached to copper surface so that copper is not by oxygen
Change, can exist steadily in the long term.
4. this conductive ink has and well puts colloidality, printing adaptability, electric conductivity and caking property；
5. this conductive ink is adapted so that and is used in paper, on pottery, glass and various plastic matrix；
6. after passing through the techniques such as ink jet printing, aerosol injection printing, intaglio printing, silk screen printing, flexible printing or some glue
Carrying out heat cure, technique is simple and can carry out ultra-large production, drastically increases production efficiency.
Accompanying drawing explanation
Fig. 1 represents the preparation method flow chart of the copper conductive ink containing graphene oxide of the embodiment of the present invention 1；
Fig. 2 represents the preparation method flow chart of the copper conductive ink containing graphene oxide of the embodiment of the present invention 3.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below the embodiments of the present invention are carried out
Detailed elaboration.Example is served only for explaining the present invention, is not intended to limit the scope of the present invention.Unless stated otherwise, originally
Percentage composition in invention refers both to weight/mass percentage composition.
Embodiment 1
The water of Hydroxylated acrylic resin, the polyvinyl alcohol of 0.5%, the ethanol of 30% and 18% by 1.5% stirs, in vacuum
Deaeration in agitator；The spherical copper powder of the 30-60nm by 25% and the commercially available graphene oxide of 25% successively add above-mentioned
In the mixture of deaeration, ultrasonic disperse, obtain the copper conductive ink containing graphene oxide, store under the cryogenic conditions of 0 DEG C～8 DEG C
Deposit.Copper conductive ink containing graphene oxide is printed as the lines of live width about 30 μm in glass matrix by ink jet printing,
Roasting 1h at 250 DEG C in ordinary sinter stove, records its resistivity less than 1.0 × 10-4Ω·cm.The conductor wire that the method makes
Road, during life-time service, copper is not oxidized, can exist steadily in the long term.
Embodiment 2
The water of Hydroxylated acrylic resin, the polyvinyl alcohol of 0.5%, the ethanol of 30% and 18% by 1.5% stirs, in vacuum
Deaeration in agitator；The spherical copper powder of the 30-60nm by 40% and the commercially available graphene oxide of 10% successively add above-mentioned
In the mixture of deaeration, ultrasonic disperse, obtain the copper conductive ink containing graphene oxide, store under the cryogenic conditions of 0 DEG C～8 DEG C
Deposit.Copper conductive ink containing graphene oxide is printed as the lines of live width about 30 μm in glass matrix by ink jet printing,
Roasting 1h at 250 DEG C in ordinary sinter stove, records its resistivity less than 1.0 × 10-4Ω·cm.The conductor wire that the method makes
Road, during life-time service, copper is not oxidized, can exist steadily in the long term.
Embodiment 3
Ternary chlorine vinegar resin by 7%, 8% mixed type hydroxy polyester resin, the copolymer in cinnamic acrylic ester of 0.5%, 1%
The DBE of castor oil hydrogenated, the polyvinyl alcohol of 0.5%, the terpineol of 10% and 3% stirs, de-in vacuum defoamation blender
Bubble；The flake copper of the 2-3 μm by 35% and the commercially available graphene oxide of 35% successively add in the mixture of above-mentioned deaeration, super
Sound disperses, and obtains graphene oxide/copper conductive mixture；Then, said mixture is ground to three rod grinders, 50 revs/min
8 dischargings of mechanical lapping under conditions of clock, store after discharging under the cryogenic conditions of 0 DEG C～8 DEG C.By screen process press by institute
Stating slurry and be printed as the lines of live width about 80 μm in glass matrix, in ordinary sinter stove, roasting 1h at 250 DEG C, records its resistance
Rate is less than 1.0 × 10-4Ω·cm.The conducting wire that the method makes, during life-time service, copper is not oxidized, can be long-term
Stable existence.
Embodiment 4
Ternary chlorine vinegar resin by 7%, 8% mixed type hydroxy polyester resin, the copolymer in cinnamic acrylic ester of 0.5%, 1%
The DBE of castor oil hydrogenated, the polyvinyl alcohol of 0.5%, the terpineol of 10% and 3% stirs, de-in vacuum defoamation blender
Bubble；The flake copper of the 2-3 m by 50% and the commercially available graphene oxide of 20% successively add in the mixture of above-mentioned deaeration, super
Sound disperses, and obtains graphene oxide/copper conductive mixture；Then, said mixture is ground to three rod grinders, 50 revs/min
8 dischargings of mechanical lapping under conditions of clock, store after discharging under the cryogenic conditions of 0 DEG C～8 DEG C.By screen process press by institute
Stating slurry and be printed as the lines of live width about 80 μm in glass matrix, in ordinary sinter stove, roasting 1h at 250 DEG C, records its resistance
Rate is less than 1.0 × 10-4Ω·cm.The conducting wire that the method makes, during life-time service, copper is not oxidized, can be long-term
Stable existence.
The step of the most various methods divides, and is intended merely to describe clear, it is achieved time can merge into a step or
Some step is split, is decomposed into multiple step, as long as comprising identical logical relation, all at the protection domain of this patent
In；To adding inessential amendment in algorithm or in flow process or introducing inessential design, but do not change its algorithm
With the core design of flow process all in the protection domain of this patent.
It will be understood by those skilled in the art that the respective embodiments described above are to realize the specific embodiment of the present invention,
And in actual applications, can to it, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.
Claims (9)
1. the copper conductive ink containing graphene oxide, it is characterised in that percentage composition by weight, the component including following:
The graphene oxide of 0.5-90%, the copper powder of 0.5-90%, the resin of 1-50%, the wetting agent of 0-1%, the thixotropic agent of 0-1%, 0.5-
1% thickening agent, the coupling agent of 0-1% and the solvent of 2-60%.
2. copper conductive ink as claimed in claim 1, it is characterised in that described graphene oxide is hydroxylating Graphene, carboxylic
Base functionalized graphene, the graphene oxide of different proportion hydroxycarboxyl group or the one of commercially available common graphene oxide or many
Kind；The more preferably mol ratio of hydroxyl and carboxyl is 1:3-3:1.
3. the copper conductive ink as described in any one of claim 1-2, it is characterised in that described graphene oxide accounts for copper conductive ink
The 30-50% of water weight, and the mass percent sum of each component is 100%；And/or, described copper powder accounts for copper conductive ink weight
30-70%, and the mass percent sum of each component is 100%.
4. the copper conductive ink as described in any one of claim 1-3, it is characterised in that described copper powder be spherical, wire and/or
Lamellar, preferably copper powder are spherical, the flake copper of a size of 1nm-20 μm, diameter 1nm-20 μm, the wire copper of length 1-50 μm
One or more in powder.
5. the preparation method of the copper conductive ink described in an any one of claim 1-4, it is characterised in that comprise following step
Rapid: by weight percent, first by the resin of 1-50%, the wetting agent of 0-1%, the thixotropic agent of 0-1%, 0.5-1% thickening agent, 0-1%
Coupling agent and the stirring solvent of 2-60% uniform, deaeration in vacuum defoamation blender；By the graphene oxide of 0.5-90%,
The copper powder of 0.5-90% successively adds in the mixture of deaeration, ultrasonic disperse；Then, optionally, by the mixing after ultrasonic disperse
Thing grinds；Store under the cryogenic conditions of 0 DEG C～8 DEG C after discharging.
6. preparation method as claimed in claim 5, it is characterised in that the grinder used in described process of lapping is that three rods grind
Grinding machine, mechanical lapping 1-10 time under conditions of 50 revs/min.
7. the using method of the copper conductive ink described in claim 1-6, it is characterised in that use the copper of above-mentioned preparation to conduct electricity
Ink is by ink jet printing, aerosol injection printing, silk screen printing, intaglio printing, flexible printing, dip-coating, some glue or is sprayed on
In paper, glass, pottery, plastics and other base, in atmospheric atmosphere, less than 250 DEG C within the temperature range of sintering after, resistivity is less than
1×10-4Ω·cm。
8., according to the application of the copper conductive ink described in claim 1-6, its feature is using it for making RFID tag
The interconnecting leads such as antenna, wearable electronic product, printed circuit board, flexible transparent electrode.
Apply the most as claimed in claim 8, it is characterised in that copper conductive ink is transferred in substrate, less than at 250 DEG C
Sintering curing becomes wire.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800833A (en) * | 2017-01-11 | 2017-06-06 | 青岛瑞利特新材料科技有限公司 | Modified copper system electrically conductive ink of a kind of Graphene and preparation method thereof |
| CN106893407A (en) * | 2017-03-06 | 2017-06-27 | 苏州圣瑞赛新材料科技有限公司 | A kind of watersoluble plumbago alkene ink-jet ink and preparation method thereof |
| WO2019143912A1 (en) * | 2018-01-19 | 2019-07-25 | Lawrence Livermore National Security, Llc | Products having sheets of 2d materials and related inks for direct ink writing |
| CN110414653A (en) * | 2018-04-28 | 2019-11-05 | 华瑞墨石丹阳有限公司 | A kind of RFID label tag and its processing method and graphene antenna |
| CN111320910A (en) * | 2020-04-15 | 2020-06-23 | 汪华衡 | Conductive coating for plastics and preparation method thereof |
| CN111334153A (en) * | 2020-04-13 | 2020-06-26 | 绍兴诺鼎卫浴洁具股份有限公司 | Heat-conducting modified polyurethane super-hydrophobic composite coating and preparation method thereof |
| CN112251077A (en) * | 2020-10-10 | 2021-01-22 | 山东华冠智能卡有限公司 | Graphene conductive ink, preparation method thereof and RFID label |
| CN114836078A (en) * | 2022-04-28 | 2022-08-02 | 山东华冠智能卡有限公司 | Anti-aging graphene conductive paste for gravure printing and preparation method thereof |
| WO2023287492A3 (en) * | 2021-05-25 | 2023-04-27 | The Research Foundation For The State University Of New York | High-temperature cu ink-based conductor with oxidation and corrosion resistance |
| WO2023199214A1 (en) * | 2022-04-12 | 2023-10-19 | Graphenaton Technologies Sa | Conductive strip |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800833A (en) * | 2017-01-11 | 2017-06-06 | 青岛瑞利特新材料科技有限公司 | Modified copper system electrically conductive ink of a kind of Graphene and preparation method thereof |
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| CN110414653B (en) * | 2018-04-28 | 2024-02-02 | 华瑞墨石丹阳有限公司 | RFID tag, processing method thereof and graphene antenna |
| CN110414653A (en) * | 2018-04-28 | 2019-11-05 | 华瑞墨石丹阳有限公司 | A kind of RFID label tag and its processing method and graphene antenna |
| CN111334153A (en) * | 2020-04-13 | 2020-06-26 | 绍兴诺鼎卫浴洁具股份有限公司 | Heat-conducting modified polyurethane super-hydrophobic composite coating and preparation method thereof |
| CN111320910A (en) * | 2020-04-15 | 2020-06-23 | 汪华衡 | Conductive coating for plastics and preparation method thereof |
| CN112251077A (en) * | 2020-10-10 | 2021-01-22 | 山东华冠智能卡有限公司 | Graphene conductive ink, preparation method thereof and RFID label |
| CN112251077B (en) * | 2020-10-10 | 2021-07-06 | 山东华冠智能卡有限公司 | Graphene conductive ink, preparation method thereof and RFID label |
| WO2023287492A3 (en) * | 2021-05-25 | 2023-04-27 | The Research Foundation For The State University Of New York | High-temperature cu ink-based conductor with oxidation and corrosion resistance |
| WO2023199214A1 (en) * | 2022-04-12 | 2023-10-19 | Graphenaton Technologies Sa | Conductive strip |
| CN114836078A (en) * | 2022-04-28 | 2022-08-02 | 山东华冠智能卡有限公司 | Anti-aging graphene conductive paste for gravure printing and preparation method thereof |
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