CN109401443A - A kind of graphene coated copper nano-particle composite material conductive ink and preparation method thereof - Google Patents
A kind of graphene coated copper nano-particle composite material conductive ink and preparation method thereof Download PDFInfo
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- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a kind of graphene coated copper nano-particle composite material conductive ink and preparation method thereof, and component is in mass ratio are as follows: 5-25 parts of conductive filler, 20-40 parts of binder, 1-5 parts of auxiliary agent, 30-60 parts of solvent.Its conductive filler is the copper nano particles of graphene coated, copper nano particles oxidation bring electric conductivity, which is overcome, by effective cladding of graphene and copper weakens and be difficult to the problems such as evenly dispersed, and the electrically conductive ink relative to metal packing system greatly reduces the dosage of metallic particles, the electrically conductive ink prepared by has good conductive property and excellent flexility.
Description
Technical field
The invention belongs to graphene composition metal nano-particles reinforcement electrically conductive ink more particularly to graphene coated copper nanometers
Composite material conductive ink and a kind of composite conducting ink for being used for thin film switch, electronic device, solar cell and radio frequency identification
And preparation method thereof.
Background technique
Conductive functional ink, that is, electrically conductive ink after printing.Silver and epoxy are prepared for early in American in 1948
The blank of the electrically conductive ink of resin mixing.Japan start to develop the 1950s silver system with antistatic neck effect and
Carbon series conductive coating.Application with electrically conductive ink in electromagnetic shielding and hot spot conversion art is gradually goed deep into, and electrically conductive ink takes
Obtained swift and violent development.Predicted 2024 according to IDTechEx company, electrically conductive ink will be widely applied to automobile, touch,
The fields such as photoelectricity, radio frequency identification, sensor, intelligent packaging, logic and memory, tax revenue are up to 2,800,000,000 dollars.Huge
Interests promote and push the rapid expansion in electrically conductive ink market, therefore develop and meet the electrically conductive inks of market particular demands and be
The task of top priority.
Conductive filler is the core component in electrically conductive ink.Electrically conductive ink can be divided mainly into nothing according to the difference of conductive filler
Machine electrically conductive ink and organic conductive inks two major classes.Inorganic can pass the printing ink of the electric current is mainly by metallic and Carbon materials as conductive
Filler preparation, metal packing have gold, silver, copper etc., and carbons filler mainly includes graphite and carbon black etc.；Organic conductive inks are mainly
It is prepared by conducting polymer, such as polyacetylene, polyphenylene ethylene, polypyrrole organic material.At present the electrically conductive ink of metal system because
Its excellent performance is widely used in electronic device.Silver electronic paste electrically conductive ink is that current commercialization degree is highest, so silver
Price height belongs to precious metal material and limits its swift and violent development.Pass of the copper as base metal with high cost performance by people
Note, but copper product is easily aoxidized in air so that reducing its electric conductivity limits it as main conductive filler in conduction
The application in the fields such as ink, additionally due to the heat-shrinkable of copper powder or copper slurry, copper starches the dispersion etc. of copper powders in preparation process
Problem is also the main reason for limiting its application.
In addition, in recent years, carbon system ink is applied to some heating circuits with cheap, such as thin film switch, solar energy
Battery etc..The Graphene conductive ink especially researched and developed in recent years by the excellent electric conductivity of graphene and its have with spray
Ink prints compatible performance and is concerned, and can satisfy the demand of electronics industry if it can improve its electric conductivity.And it is based on stone
The raising of the toughness of the introducing bring resin of black alkene, promotes the anti-crawl agentdefiection folding endurance of ink, is conducive to answering on a flexible substrate
With.
Summary of the invention
The present invention provides a kind of graphene coated copper nano-particle nanocomposite electrically conductive ink and preparation method thereof,
With solve existing ink electric conductivity and excellent flexible technical problem.
The present invention provides a kind of graphene coated copper nano-particle nanocomposite electrically conductive ink, the graphene packets
Copper nano-particle nanocomposite electrically conductive ink is covered by 5-25 parts of conductive filler, 20-40 parts of binder, 1-5 parts of auxiliary agent and molten
30-60 parts of doping of agent are prepared.
Preferably, the conductive filler is the copper nano particles of graphene coated.
Preferably, the binder be ethyl cellulose, polyurethane resin, epoxy resin E-51, epoxy resin E-44,
Cellulose acetate-butyrate, cellaburate gather intoxicated gum resin, acrylic resin, pass through main propyl methocel, ternary chlorine acetic acid
It is one or more of in resin.
Preferably, the solvent is organic solvent.
Preferably, the organic solvent is ethyl alcohol, ethylene glycol, isopropanol, terpinol, the third blue alcohol, hexadecanol, mixed diacid two
First vinegar, hexamethylene be intoxicated, acetic acid ethyl ester, bluff E from sour diformazan vinegar, positive third vinegar of propylene glycol, propylene glycol first enzyme acetic acid vinegar, propylene glycol first vinegar,
One or more of the positive fourth vinegar of glutaric acid diformazan vinegar, acetic acid, adipic acid diformazan vinegar, lauryl alcohol vinegar.
Preferably, the auxiliary agent be one of dispersing agent, curing agent, defoaming agent, delustering agent, thixotropic agent, stabilizer or
It is several.
A kind of preparation method of the copper nano particles of graphene coated, it is characterised in that the method comprises the following steps:
(1) by copper chloride (CuCl2) and reducing agent solution be added beaker in and stir；
(2) increase dispersing agent, mixed solution toward step (1) and stir；
(3) it will be warming up to 80 ~ 220 degrees Celsius in liquid placing response kettle obtained in step (2) and keep the temperature 8 ~ 16 hours
The nanocomposite of graphene coated copper nano particles is prepared.
Preferably, the reducing agent is one or more of ascorbic acid, citric acid；The dispersing agent is polyethylene pyrrole
Pyrrolidone；The molten mixing is the mixed liquor for being dissolved in graphene oxide and ethylene glycol.
A kind of graphene coated copper nano-particle nanocomposite electrically conductive ink preparation method, it is characterised in that the side
Steps are as follows for method:
(1) 20-40 parts of binders are dissolved in 30-60 parts of solvents and are mixed and stirred for, can be obtained after binder all dissolution
Binder mixed liquor；
(2) ball milling in ball grinder is added in 1-5 parts of auxiliary agents and 5-25 parts of conductive fillers and carries out ball milling, Ball-milling Time is 0.1 ~ 1h；
(3) step (1) obtained binder mixed liquor is added into step (2), and continues ball milling 0.1 ~ can be obtained lead for 24 hours
Plasma-based material；
(4) step (3) obtained electrocondution slurry is filtered packing can be obtained receiving for graphene coated copper nano particles
Rice composite conducting ink.
Preferably, the mill speed is 150 ~ 550rpm.
Compared with prior art, the present invention the present invention most has the advantages that:
1) use the copper nano particles of graphene coated for conductive filler.By the cladding of graphene, it is improved copper nanometer
The antioxygenic property of grain inhibits its reunion performance.In conjunction with the strong mechanical performance of grapheme material and bigger serface, have
The electric conductivity for improving electrically conductive ink obtained of effect, flexibility and stability.
2) connecting hydro-thermal reaction restores graphene oxide (GO) under conditions of moderate notoxic as redox
Graphene (rGO), and be coated on copper nano particles surface and form nanocomposite.I.e. by simple hydro-thermal reaction, with low
Effective anti-oxidant modification of the realization at low cost to copper product, effectively inhibits the reunion of copper nano particles, improves copper nanometer
The antioxygenic property of particle.
3) copper nano particles and graphene are constituted is conductively connected network well, improves the electric conductivity of electrically conductive ink and soft
Tough performance.By the viscosity and thixotropy of the adjustable electrically conductive ink of composition regulation, there is electrically conductive ink better
Electric conductivity and easily disperse can also improve the printing performance of ink.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below with reference to embodiment to skill of the invention
Art scheme is further described, and however, it is not limited to this, and all modifying or equivalently replacing the technical solution of the present invention,
Without departing from the spirit and scope of the technical solution of the present invention, should all cover within the protection scope of the present invention.
The embodiment of the invention discloses a kind of graphene coated copper nano-particle nanocomposite electrically conductive ink, the stones
Black alkene cladding copper nano-particle nanocomposite electrically conductive ink is by 5-25 parts of conductive filler, 20-40 parts of binder, auxiliary agent 1-5
Part and solvent 30-60 parts of doping are prepared.
Further, the conductive filler is the copper nano particles of graphene coated.The wherein copper nanometer of graphene coated
Preparation method of granules are as follows: with copper chloride (CuCl2) it is presoma, it is also with ascorbic acid and citric acid one of which or mixture
Former agent is dissolved in the mixed solution of graphene oxide and ethylene glycol, then they is moved to using polyvinylpyrrolidone as dispersing agent
It is warming up to 100 ~ 150 degrees Celsius in reaction kettle and keeps the temperature 12 hours, it can receiving for graphene coated copper nano particles is prepared
Nano composite material.The particle size distribution range for the copper nano particles for using this method to prepare for 30-150nm(according to reducing agent and
The content of hydrothermal temperature and GO are adjustable), and they and redox graphene are compound uniformly.This graphene coated copper nanometer
The reunion that particle (Cu NPs@rGO) effectively inhibits copper nano particles increases its dispersibility, effectively inhibits and is received by Cu
Rice grain be directly exposed to air caused by surface oxidation bring electric conductivity reduction.Furthermore the strong machinery of graphene
Performance, flexibility and big specific surface area increase the flexibility of final electrically conductive ink and the adhewsive action of itself and substrate.
A kind of graphene coated copper nano-particle nanocomposite electrically conductive ink preparation method is to take quota conductive filler
5-25 parts, 20-40 parts of binder, 1-5 parts of auxiliary agent, 30-60 parts of solvent.Wherein conductive filler of the invention is to be made in the present invention
Cu NPs@rGO nanocomposite；Binder is that high molecular material (can be selected from ethyl cellulose, polyurethane tree
Rouge, epoxy resin E-44, cellulose acetate-butyrate, cellaburate, gathers intoxicated gum resin, acrylic acid tree at epoxy resin E-51
Rouge one or more of passes through main propyl methocel, ternary chlorine vinegar acid resin etc.).Solvent is that organic solvent (can be selected from second
Alcohol, ethylene glycol, isopropanol, terpinol, the third blue alcohol, hexadecanol, mixed diacid diformazan vinegar, hexamethylene are intoxicated, acetic acid ethyl ester, bluff E from acid two
Positive third vinegar of first vinegar, propylene glycol, propylene glycol first enzyme acetic acid vinegar, propylene glycol first vinegar, glutaric acid diformazan vinegar, the positive fourth vinegar of acetic acid, adipic acid
One or more of diformazan vinegar, lauryl alcohol vinegar etc.).Auxiliary agent in the present invention can be selected from dispersing agent, curing agent, defoaming agent, disappear
One or more of photo etching, thixotropic agent, stabilizer etc..And the binder of selected share will be dissolved in the solvent of selected share
It is mixed, binder mixed liquor can be obtained after binder all dissolution.Then the auxiliary agent of selected share and specific part
The conductive filler (Cu NPs@rGO) of volume is added in ball grinder after 0.1 ~ 1h of ball milling, add binder mixed liquor ball milling 0.1 ~
Electrocondution slurry can be obtained in (mill speed of preferred settings is between 150 ~ 550rpm) for 24 hours.Finally electrocondution slurry was carried out
The nano combined electrically conductive ink of graphene coated copper nano particles can be obtained in filter packing.
Example one:
A kind of technology of preparing of graphene coated copper nano-particle (Cu NPs@rGO) nanocomposite electrically conductive ink is by graphite
15 parts of alkene coated copper nanocomposite be used as conductive filler, 35 parts of polyamide be binder, with stabilizer, delustering agent,
Curing agent and thixotropic agent press 5 parts of mixed aid of the mass ratio composition of 2:1:1:1, with propylene glycol first vinegar and ethylene glycol glutaric acid
Diformazan vinegar presses 45 parts of mixed solvent of the mass ratio composition of 1:1.5.
Cu NPs@rGO nanocomposite in the example uses CuCl2For presoma, using ascorbic acid as reducing agent,
Using polyvinylpyrrolidone as dispersing agent, it is dissolved in the mixed solution of graphene oxide and ethylene glycol, they are then moved to reaction
It is warming up in kettle made from 120 degrees Celsius of heat preservations 12 hours, the partial size of copper nano particles is 80 ~ 120 nm.
The binder of above-mentioned share is dissolved in the solvent of above-mentioned share and mixes to all dissolutions and obtain binder and mix
Close liquid.0.2 h of ball milling in ball grinder is added in the auxiliary agent of above-mentioned share and the Cu NPs@rGO nanocomposite of above-mentioned share
Afterwards, it adds the mill speed that binder mixed liquor ball milling 15h(is set and obtains electrocondution slurry as 500rpm).Finally by conductive paste
Material, which is filtered packing, can be obtained the nano combined electrically conductive ink of graphene coated copper nano particles.
Example two:
A kind of technology of preparing of graphene coated copper nano-particle (Cu NPs@rGO) nanocomposite electrically conductive ink is by graphite
15 parts of alkene coated copper nanocomposite are used as conductive filler, using 5 parts of acidification carbon fibers and 35 parts of epoxy resin as binder, with
Stabilizer, curing agent and thixotropic agent by 2:1:0.5 mass ratio form 3 parts of mixed aid, with 15 parts of ethyl alcohol, 5 parts of acetone and
The mixed solvent of 22 parts of dipropylene glycols composition.
Cu NPs@rGO nanocomposite in the example uses CuCl2For presoma, with ascorbic acid and citric acid
(1:1) is dissolved in the mixed solution of graphene oxide and ethylene glycol, then using polyvinylpyrrolidone as dispersing agent for reducing agent
They are moved in reaction kettle and is warming up to made from 110 degrees Celsius of heat preservations 12 hours, the partial size of copper nano particles is 50 ~ 90
nm。
The binder of above-mentioned share is dissolved in the solvent of above-mentioned share and mixes to all dissolutions and obtain binder and mix
Close liquid.0.2 h of ball milling in ball grinder is added in the auxiliary agent of above-mentioned share and the Cu NPs@rGO nanocomposite of above-mentioned share
Afterwards, it adds the mill speed that binder mixed liquor ball milling 15h(is set and obtains electrocondution slurry as 500rpm).Finally by conductive paste
Material, which is filtered packing, can be obtained the nano combined electrically conductive ink of graphene coated copper nano particles.
Example three:
A kind of technology of preparing of graphene coated copper nano-particle (Cu NPs@rGO) nanocomposite electrically conductive ink is by graphite
15 parts of alkene coated copper nanocomposite are used as conductive filler, using 5 parts of acidification carbon fibers, 30 parts of epoxy resin as binder, with
Stabilizer, defoaming agent, delustering agent, curing agent and thixotropic agent press 5 parts of mixed aid of the mass ratio composition of 2:1:1:0.5:0.5,
The mixed solvent formed with 10 parts of ethylene glycol, 5 parts of acetone and 25 parts of dipropylene glycols.
Cu NPs@rGO nanocomposite in the example uses CuCl2For presoma, using citric acid as reducing agent, with
Polyvinylpyrrolidone is dispersing agent, is dissolved in the mixed solution of graphene oxide and ethylene glycol, they are then moved to reaction kettle
In be warming up to made from 120 degrees Celsius of heat preservations 12 hours, the partial sizes of copper nano particles is 80 ~ 150 nm.
The binder of above-mentioned share is dissolved in the solvent of above-mentioned share and mixes to all dissolutions and obtain binder and mix
Close liquid.0.4 h of ball milling in ball grinder is added in the auxiliary agent of above-mentioned share and the Cu NPs@rGO nanocomposite of above-mentioned share
Afterwards, it adds the mill speed that binder mixed liquor ball milling 20h(is set and obtains electrocondution slurry as 500rpm).Finally by conductive paste
Material, which is filtered packing, can be obtained the nano combined electrically conductive ink of graphene coated copper nano particles.
By electrically conductive ink that the compound copper nano particles of graphene obtained above are filler using PET plastic film as substrate, make
With the halftone of 200 mesh, silk-screen printing is carried out, then is dried at room temperature for solidification 30min, is finally obtained with a thickness of 10 μm or so
Cured composite conducting ink film, tests it, as a result as follows:
| Performance indicator | Common conductive ink | Example 1 | Example 2 | Example 3 |
| Thickness (μm) | 25 | 10 | 10 | 10 |
| Adhesive force | 1 grade | 0 grade, doubling is without mark of break | 0 grade, doubling is without mark of break | 0 grade, doubling is without mark of break |
| Hardness | H | 2H | 3H | 2H |
| Sheet resistance (m Ω) | 50 | 20 | 22 | 25 |
Therefore graphene coated copper nano-particle composite material conductive ink is substantially better than common conductive ink.
By electrically conductive ink that the compound copper nano particles of graphene obtained above are filler using PVC plastic film as substrate, make
With flexographic printing, then the baking and curing 30min at 70 DEG C, finally obtains the cured composite conducting oil with a thickness of 3 μm or so
Ink film tests it, as a result as follows:
In conclusion cladding of the present invention by graphene, the antioxygenic property for being improved copper nano particles inhibits its
Reunion performance, while in conjunction with the strong mechanical performance of grapheme material and bigger serface, effectively raise conduction obtained
The electric conductivity of ink, flexibility and stability；Simple hydro-thermal reaction is crossed, is realized so that low cost is low to the effective anti-of copper product
Oxidative modification effectively inhibits the reunion of copper nano particles, improves the antioxygenic property of copper nano particles；Copper nano particles
It is constituted with graphene and is conductively connected network well, improve the electric conductivity and flexility of electrically conductive ink.Pass through composition regulation
The viscosity and thixotropy of adjustable electrically conductive ink not only make electrically conductive ink have better electric conductivity and easily disperse, also
The printing performance of ink can be improved.
Finally it should be noted that the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
Invention is explained in detail referring to above-described embodiment for pipe, it should be understood by a person of ordinary skill in the art that technology
Personnel read present specification after still can with modifications or equivalent substitutions are made to specific embodiments of the invention, but this
A little modifications are changed within all without departing from the present patent application accompanying claims protection scope.
Claims (10)
1. a kind of graphene coated copper nano-particle composite material conductive ink, which is characterized in that the graphene coated copper is received
Rice corpuscles nanocomposite electrically conductive ink is by 5-25 parts of conductive filler, 20-40 parts of binder, 1-5 parts of auxiliary agent and solvent 30-60
Part doping is prepared.
2. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 1, which is characterized in that
The conductive filler is the copper nano particles of graphene coated.
3. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 1, which is characterized in that
The binder be ethyl cellulose, polyurethane resin, epoxy resin E-51, epoxy resin E-44, cellulose acetate-butyrate,
Cellaburate gathers intoxicated gum resin, acrylic resin, passes through main propyl methocel, is a kind of or several in ternary chlorine vinegar acid resin
Kind.
4. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 1, which is characterized in that
The solvent is organic solvent.
5. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 4, which is characterized in that
The organic solvent is that ethyl alcohol, ethylene glycol, isopropanol, terpinol, the third blue alcohol, hexadecanol, mixed diacid diformazan vinegar, hexamethylene be intoxicated, second
Sour second vinegar bluffs E from sour diformazan vinegar, positive third vinegar of propylene glycol, propylene glycol first enzyme acetic acid vinegar, propylene glycol first vinegar, glutaric acid diformazan vinegar, second
One or more of sour positive fourth vinegar, adipic acid diformazan vinegar, lauryl alcohol vinegar.
6. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 1, which is characterized in that
The auxiliary agent is one or more of dispersing agent, curing agent, defoaming agent, delustering agent, thixotropic agent, stabilizer.
7. a kind of preparation method of the copper nano particles of graphene coated described in claim 1-6 any claim, feature
Be the method comprises the following steps:
(1) by copper chloride (CuCl2) and reducing agent solution be added beaker in and stir；
(2) increase dispersing agent, mixed solution toward step (1) and stir；
(3) it will be warming up to 80 ~ 220 degrees Celsius in liquid placing response kettle obtained in step (2) and keep the temperature 8 ~ 16 hours
The nanocomposite of graphene coated copper nano particles is prepared.
8. a kind of graphene coated copper nano-particle composite material conductive ink according to claim 7, which is characterized in that
The reducing agent is one or more of ascorbic acid, citric acid；The dispersing agent is polyvinylpyrrolidone；The mixing
Molten is the mixed liquor for being dissolved in graphene oxide and ethylene glycol.
9. prepared by graphene coated copper nano-particle composite material conductive ink described in a kind of claim 1-8 any claim
Method, it is characterised in that the method comprises the following steps:
(1) 20-40 parts of binders are dissolved in 30-60 parts of solvents and are mixed and stirred for, can be obtained after binder all dissolution
Binder mixed liquor；
(2) ball milling in ball grinder is added in 1-5 parts of auxiliary agents and 5-25 parts of conductive fillers and carries out ball milling, Ball-milling Time is 0.1 ~ 1h；
(3) step (1) obtained binder mixed liquor is added into step (2), and continues ball milling 0.1 ~ can be obtained lead for 24 hours
Plasma-based material；
(4) step (3) obtained electrocondution slurry is filtered packing can be obtained receiving for graphene coated copper nano particles
Rice composite conducting ink.
10. graphene coated copper nano-particle nanocomposite electrically conductive ink preparation method according to claim 9,
It is characterized in that, the mill speed is 150 ~ 550rpm.
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| CN110862716A (en) * | 2019-12-18 | 2020-03-06 | 九江纳维新材料科技有限公司 | Graphene composite conductive ink and preparation method thereof |
| CN111393910A (en) * | 2020-05-11 | 2020-07-10 | 南昌航空大学 | Composite nano-copper conductive ink, preparation method thereof and conductive device |
| CN111849253A (en) * | 2020-08-07 | 2020-10-30 | 河南墨特石墨烯科技有限公司 | Graphene heating water-based ink and preparation method thereof |
| CN112185623A (en) * | 2020-09-28 | 2021-01-05 | 东莞记忆存储科技有限公司 | Preparation process and packaging application of graphene-coated nano copper slurry |
| CN112375270A (en) * | 2020-11-11 | 2021-02-19 | 珠海京工检测技术有限公司 | Conductive rubber for electronic packaging and preparation method thereof |
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| CN114958074A (en) * | 2022-05-18 | 2022-08-30 | 广东墨睿科技有限公司 | Graphene conductive ink and preparation method thereof |
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| CN110862716A (en) * | 2019-12-18 | 2020-03-06 | 九江纳维新材料科技有限公司 | Graphene composite conductive ink and preparation method thereof |
| CN111393910A (en) * | 2020-05-11 | 2020-07-10 | 南昌航空大学 | Composite nano-copper conductive ink, preparation method thereof and conductive device |
| CN111849253A (en) * | 2020-08-07 | 2020-10-30 | 河南墨特石墨烯科技有限公司 | Graphene heating water-based ink and preparation method thereof |
| CN112185623A (en) * | 2020-09-28 | 2021-01-05 | 东莞记忆存储科技有限公司 | Preparation process and packaging application of graphene-coated nano copper slurry |
| CN112185623B (en) * | 2020-09-28 | 2022-06-07 | 东莞记忆存储科技有限公司 | Preparation process and packaging application of graphene-coated nano copper slurry |
| CN112375270A (en) * | 2020-11-11 | 2021-02-19 | 珠海京工检测技术有限公司 | Conductive rubber for electronic packaging and preparation method thereof |
| CN113053557A (en) * | 2021-03-09 | 2021-06-29 | Tcl华星光电技术有限公司 | Conductive electrode material, preparation method thereof and conductive electrode |
| CN114958074A (en) * | 2022-05-18 | 2022-08-30 | 广东墨睿科技有限公司 | Graphene conductive ink and preparation method thereof |
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Application publication date: 20190301 |