CN108485382A - A method of preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver - Google Patents
A method of preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver Download PDFInfo
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- CN108485382A CN108485382A CN201810547573.4A CN201810547573A CN108485382A CN 108485382 A CN108485382 A CN 108485382A CN 201810547573 A CN201810547573 A CN 201810547573A CN 108485382 A CN108485382 A CN 108485382A
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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
- C09D11/10—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
Abstract
The invention discloses a kind of methods preparing graphene-based conductive ink with multi-walled carbon nanotube nano silver, it is characterized in that, the concentrated sulfuric acid and concentrated nitric acid are mixed, add wall carbon nano tube, temperature constant magnetic stirring flows back, it is neutrality to be diluted with water to pH value of solution, filters, is dried in vacuo to obtain carboxylic carbon nano-tube suspension；Into polyvinylpyrrolidone plus water stirs, and prepares dispersant solution, carboxylic carbon nano-tube suspension is added, ultrasonic disperse obtains carbon nano tube suspension；Into silver oxalate plus deionized water is uniformly dispersed, and ammonium hydroxide is added dropwise and adjusts pH, adds structure inducer, is transferred in polyethylene plastic bag, seals, is irradiated by radiation source of electron accelerator, through being evaporated under reduced pressure, being concentrated to give nano-silver powder suspension after logical nitrogen deoxygenation gas；Epoxy resin, amine epoxy resin curing agent, graphene are mixed, front resulting material is added, acetone is added to dilute, heating stirring after heating stirring, then ultrasonic vibration, obtains graphene-based conductive ink after ultrasonic vibration processing.
Description
Technical field
The present invention relates to conductive ink fields, and in particular to it is a kind of with multi-walled carbon nanotube-nano silver prepare it is graphene-based
The method of conductive ink.
Background technology
With the rapid progress of electronics technology and the increasingly raising of people's living standard, electronics industry has welcome new one
Wheel flourishes, and people propose frivolous, flexibility requirement for novel electronic product.Rely on science and technology development with
And the demand in market, printed electronic industry gradually develop into rising industry, and low cost may be implemented, large area, rapidly make
The flexibility electronic product of standby a new generation, has considerable development prospect.Printed electronic ink is to constitute printed electronic material
The important component of material, the development of printing ink are the key points of printed electronic Materials.Metallic conduction ink is with it
Manufacturing process, the good application prospect of excellent conductivity, simplicity, become the research emphasis of printed conductive ink.In green
Under the Economic Development Mode of environmental protection, Search green chemistry has become inevitable trend, this also requires printing ink gradually to turn to
Water-based system.
Invention content
The invention mainly solves the technical problem of providing a kind of graphene-based lead is prepared with multi-walled carbon nanotube-nano silver
The method of electric ink has excellent electric conductivity, heat resistance according to conductive ink prepared by the technique, and can reach good
Good solid state.
A method of preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver, which is characterized in that by following
Step carries out：
（1）The dispersion of carbon nanotube：
The 50-60 parts of concentrated sulfuric acids and 16-20 parts of concentrated nitric acids are mixed, 0.5-1 parts of multi-walled carbon nanotubes are added, in 60-63 DEG C of constant temperature
Lower heating magnetic agitation reflux 5-6h is filtered, with deionized water dilute solution pH to neutrality in 60-63 DEG C of vacuum drying chamber
Dry 20-24h, obtains carboxylic carbon nano-tube suspension；
Deionized water is added into 0.1-0.2 parts of surfactant polyvinylpyrrolidones, it is molten to prepare dispersant for mechanical agitation
Liquid, is added carboxylic carbon nano-tube suspension, and ultrasonic disperse 2-3h obtains carbon nano tube suspension；
（2）Radiation reduction method prepares nano-silver powder：
500-600 parts of deionized waters are added into 1-2 parts of silver oxalates to be uniformly dispersed, it is 8.5-9.5 that ammonium hydroxide, which is added dropwise, and adjusts pH, is added
3-6 parts of structure inducers, are transferred in polyethylene plastic bag, are sealed after logical nitrogen deoxygenation gas, using electron accelerator as radiation source
2-3min is irradiated, through 40-43 DEG C of vacuum distillation, concentration, obtains nano-silver powder suspension；
（3）The preparation of graphene-based conductive ink：
E20,20-30 parts of amine epoxy resin curing agent of 90-100 parts of epoxy resin, 20-24 parts of graphenes are mixed, are added
(1), resulting material in (2), then 200-240 parts of acetone is added to be diluted, 30-35min is handled with ultrasonic oscillation, is then heated
30-35min is handled to 90-92 DEG C of stirring 25-30min, then ultrasonic vibration, finally heated to 90-92 DEG C stirring 55-65min is obtained
To graphene-based conductive ink.
Wherein, step（1）A concentration of 0.8-0.9g/L of middle polyvinylpyrrolidone.
Step（2）Middle structure inducer is organic amine compound CS005.
The reaction mechanism of the present invention is as follows：
Concentrated sulfuric acid concentrated nitric acid nitration mixture oxidation multi-wall carbon nano-tube tube is first used, so that its surface is taken the hydrophilic radicals such as carboxyl, prepares carboxylic
The carbon nanotube of base prepares carbon nano tube suspension using surfactant polyvinylpyrrolidone as dispersant, with electronics plus
Fast device is radiation source, silver oxalate is silver-colored source, and nano-silver powder is prepared for by radiation reduction method, with graphene, multi-walled carbon nanotube,
Nano-silver powder is conductive filler, and epoxy blend is compound is prepared for graphene-based conductive ink；Graphene-based conductive ink
Have preferable adhesive force and preferable chemical resistance, while there is good heat resistance, mechanical property, fracture strength, and
And good solid state can be reached；The ink have good dispersion stabilization, excellent conductivity after solidification, with matrix have compared with
Strong adhesive force.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment
A method of preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver, which is characterized in that by following
Step carries out：
（1）The dispersion of carbon nanotube：
The 50kg concentrated sulfuric acids and 16kg concentrated nitric acids are mixed, 0.5kg multi-walled carbon nanotubes are added, magnetic is heated at 60-63 DEG C of constant temperature
Power is stirred at reflux 5h, with deionized water dilute solution pH to neutrality, filters, and dry 20h, obtains in 60-63 DEG C of vacuum drying chamber
To carboxylic carbon nano-tube suspension；
Deionized water is added into 0.1kg surfactant polyvinylpyrrolidones, mechanical agitation prepares dispersant solution, adds
Enter carboxylic carbon nano-tube suspension, ultrasonic disperse 2h obtains carbon nano tube suspension；
（2）Radiation reduction method prepares nano-silver powder：
500kg deionized waters are added into 1kg silver oxalates to be uniformly dispersed, it is 8.5-9.5 that ammonium hydroxide, which is added dropwise, and adjusts pH, and 3kg knots are added
Structure derivant, is transferred in polyethylene plastic bag, seals after logical nitrogen deoxygenation gas, is irradiated by radiation source of electron accelerator
3min obtains nano-silver powder suspension through 40-43 DEG C of vacuum distillation, concentration；
（3）The preparation of graphene-based conductive ink：
90kg epoxy resin E20,20kg amine epoxy resins curing agent, 20kg graphenes are mixed, gained in (1), (2) is added
Material, then 200kg acetone is added to be diluted, 30min is handled with ultrasonic oscillation, is then heated to 90-92 DEG C of stirring 25min,
Ultrasonic vibration handles 35min again, and finally heated to 90-92 DEG C stirring 55min obtains graphene-based conductive ink.
Wherein, step（1）A concentration of 0.8g/L of middle polyvinylpyrrolidone.
Step（2）Middle structure inducer is organic amine compound CS005.
Claims (4)
1. a kind of method preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver, which is characterized in that by the concentrated sulfuric acid
It is mixed with concentrated nitric acid, adds wall carbon nano tube, temperature constant magnetic stirring reflux, it is neutrality to be diluted with water to pH value of solution, is filtered, vacuum
Dry carboxylic carbon nano-tube suspension；Into polyvinylpyrrolidone plus water stirs, and prepares dispersant solution, carboxyl is added
Carbon nano tube suspension, ultrasonic disperse obtain carbon nano tube suspension；Into silver oxalate plus deionized water is uniformly dispersed, and ammonia is added dropwise
Water adjusts pH, adds structure inducer, is transferred in polyethylene plastic bag, is sealed after logical nitrogen deoxygenation gas, is with electron accelerator
Radiation source irradiates, through being evaporated under reduced pressure, being concentrated to give nano-silver powder suspension；By epoxy resin, amine epoxy resin curing agent, graphite
Alkene mixes, and front resulting material is added, acetone is added to dilute, and adds after heating stirring after ultrasonic vibration processing, then ultrasonic vibration processing
Thermal agitation obtains graphene-based conductive ink.
2. a kind of method preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver according to claim 1,
It is characterized in that, carrying out according to the following steps：
（1）The dispersion of carbon nanotube：
The 50-60 parts of concentrated sulfuric acids and 16-20 parts of concentrated nitric acids are mixed, 0.5-1 parts of multi-walled carbon nanotubes are added, in 60-63 DEG C of constant temperature
Lower heating magnetic agitation reflux 5-6h is filtered, with deionized water dilute solution pH to neutrality in 60-63 DEG C of vacuum drying chamber
Dry 20-24h, obtains carboxylic carbon nano-tube suspension；
Deionized water is added into 0.1-0.2 parts of surfactant polyvinylpyrrolidones, it is molten to prepare dispersant for mechanical agitation
Liquid, is added carboxylic carbon nano-tube suspension, and ultrasonic disperse 2-3h obtains carbon nano tube suspension；
（2）Radiation reduction method prepares nano-silver powder：
500-600 parts of deionized waters are added into 1-2 parts of silver oxalates to be uniformly dispersed, it is 8.5-9.5 that ammonium hydroxide, which is added dropwise, and adjusts pH, is added
3-6 parts of structure inducers, are transferred in polyethylene plastic bag, are sealed after logical nitrogen deoxygenation gas, using electron accelerator as radiation source
2-3min is irradiated, through 40-43 DEG C of vacuum distillation, concentration, obtains nano-silver powder suspension；
（3）The preparation of graphene-based conductive ink：
E20,20-30 parts of amine epoxy resin curing agent of 90-100 parts of epoxy resin, 20-24 parts of graphenes are mixed, are added
(1), resulting material in (2), then 200-240 parts of acetone is added to be diluted, 30-35min is handled with ultrasonic oscillation, is then heated
30-35min is handled to 90-92 DEG C of stirring 25-30min, then ultrasonic vibration, finally heated to 90-92 DEG C stirring 55-65min is obtained
To graphene-based conductive ink.
3. a kind of method preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver according to claim 2,
It is characterized in that, step（1）A concentration of 0.8-0.9g/L of middle polyvinylpyrrolidone.
4. a kind of method preparing graphene-based conductive ink with multi-walled carbon nanotube-nano silver according to claim 2,
It is characterized in that, step（2）Middle structure inducer is organic amine compound CS005.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110885079A (en) * | 2018-09-11 | 2020-03-17 | 天津大学 | Preparation method of novel graphene-carbon nanotube composite material |
| CN111529705A (en) * | 2020-04-28 | 2020-08-14 | 天津大学 | Preparation method of bacteriophage-CuNPs @ MWCNTs |
| CN112375432A (en) * | 2020-11-17 | 2021-02-19 | 安徽理工大学 | Carbon nanotube nano-silver conductive ink |
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| CN104650652A (en) * | 2013-11-22 | 2015-05-27 | 苏州冷石纳米材料科技有限公司 | Nano-silver conductive ink and preparation method thereof |
| CN105001716A (en) * | 2015-06-30 | 2015-10-28 | 中国科学院山西煤炭化学研究所 | Graphene-based low resistance conductive printing ink and preparation method thereof |
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2018
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| CN104650652A (en) * | 2013-11-22 | 2015-05-27 | 苏州冷石纳米材料科技有限公司 | Nano-silver conductive ink and preparation method thereof |
| CN105001716A (en) * | 2015-06-30 | 2015-10-28 | 中国科学院山西煤炭化学研究所 | Graphene-based low resistance conductive printing ink and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885079A (en) * | 2018-09-11 | 2020-03-17 | 天津大学 | Preparation method of novel graphene-carbon nanotube composite material |
| 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 |
| CN111529705A (en) * | 2020-04-28 | 2020-08-14 | 天津大学 | Preparation method of bacteriophage-CuNPs @ MWCNTs |
| CN112375432A (en) * | 2020-11-17 | 2021-02-19 | 安徽理工大学 | Carbon nanotube nano-silver conductive ink |
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