CN107298901A - A kind of carbon series conductive ink - Google Patents
A kind of carbon series conductive ink Download PDFInfo
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- CN107298901A CN107298901A CN201710751355.8A CN201710751355A CN107298901A CN 107298901 A CN107298901 A CN 107298901A CN 201710751355 A CN201710751355 A CN 201710751355A CN 107298901 A CN107298901 A CN 107298901A
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- agent
- conductive ink
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- carbon series
- curing agent
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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
Abstract
A kind of carbon series conductive ink, is related to electrically conductive ink.The component of the carbon series conductive ink is in mass ratio：Conductive filler 5~40, binding agent 2~20, curing agent 0.1~8, auxiliary agent 0.1~10, solvent 20~80；The conductive filler includes component one and component two, the component one is expanded graphite, the component two is at least one of graphene, graphite, conductive carbon fibre, CNT, conductive black, acetylene black etc., and the mass ratio of the component one and component two is (0.1~10) ︰ 1.During preparation, solvent is mixed with binding agent, until obtaining transparent binding agent mixed liquor；After expanded graphite ball milling, conductive filler, binding agent mixed liquor, curing agent and auxiliary agent are added, continues ball milling, obtains slurry；Carbon series conductive ink will be produced after slurries filtration.
Description
Technical field
The present invention relates to electrically conductive ink, more particularly, to a kind of low-temperature curable, low-resistance carbon series conductive ink and its
Preparation method.
Background technology
Traditional typography is applied to the manufacture of electronic product, this kind of novel process technology of printed electronic is expanded out,
It has the trend to flexible, low cost, environmental protection and high-performance development, and electrically conductive ink is the pass of printed electronics
Key.At present, nano metal electrically conductive ink, especially silver-colored electrically conductive ink, which is widely used in conductive electrode, opto-electronic device, radio frequency, to be known
Not, the flexible electronic such as biology sensor field.For nano metal electrically conductive ink, the cost advantage of carbon series conductive ink is dashed forward
Go out, moreover it is possible to compatible with inkjet printing mode, the ink film layer printed out is difficult oxidation, performance is stable, acid and alkali resistance and change after solidification
Learn solvent corrosion.But its electric conductivity is general, existing market is badly in need of class low cost, the carbon series conductive oil with superior electrical conductivity
Ink.
High-quality electrically conductive ink requires that printability is good, solidification temperature is low, adhesive force is strong, rate of drying is fast, resistivity
Low, hardening time is short, electric conductivity is stable.Particularly RFID antenna is typically printed on flexible parent metal, such as PET, paper, right
Flexibility requirements after electrically conductive ink solidification are higher.Low-temperature short-time solidify except energy consumption can be reduced, moreover it is possible to expand ink intolerant to
Application on high temperature substrate, is also the trend place of ink development from now on.
The content of the invention
It is an object of the invention to solve the above-mentioned problems in the prior art, there is provided the conduction that can lift carbon system ink
Property, the anti-crawl agentdefiection folding endurance of ink diaphragm is improved to resin toughening, ink solidification temperature is substantially reduced, and it is easy to long-term preservation, it can solve
Certainly in ink expanded graphite introducing technique, improve a kind of carbon series conductive ink and preparation method thereof of grinding efficiency.
The component of the carbon series conductive ink is in mass ratio：
Conductive filler 5~40, binding agent 2~20, curing agent 0.1~8, auxiliary agent 0.1~10, solvent 20~80；It is described to lead
Electric filler includes component one and component two, and the component one is expanded graphite, and the component two is graphene, graphite, conductive carbon
The mass ratio of at least one of fiber, CNT, conductive black, acetylene black etc., the component one and component two is (0.1
~10) ︰ 1.
The binding agent may be selected from epoxy resin, acrylic resin, ternary chlorine vinegar acid resin, polyurethane resin, polyamide
At least one of resin etc..
The curing agent may be selected from least one of amine curing agent, imidazole curing agent, acid anhydride type curing agent etc..
The amine curing agent may be selected from urea, ethylenediamine, triethylene tetramine, m-phenylene diamine (MPD), polyamide, cdicynanmide etc.
At least one.
The imidazole curing agent may be selected from 1,3- methylimidazoles salt compounded of iodine, 2-ethyl-4-methylimidazole, 2-methylimidazole
At least one of Deng.
It is adjacent that the acid anhydride type curing agent may be selected from methylnadic anhydride, methyl tetrahydrophthalic anhydride, methyl hexahydro
At least one of phthalate anhydride etc..
The curing agent includes curing accelerator, and the mass percentage content of the curing accelerator is curing agent
0.01%~10%；The curing accelerator may be selected from benzyl dimethylamine, dimethylamino cresols, DMP-10, DMP-20, DMP-30
At least one of Deng.
The auxiliary agent may be selected from dispersant, stabilizer, film forming agent, coupling agent, plasticizer, defoamer, thickener, levelling
At least one of agent, thixotropic agent etc..
The solvent may be selected from methanol, ethanol, n-butanol, isobutanol, terpinol, isopropanol, glycerine, ethyl acetate,
Cyclohexanone, butanone, isophorone, n-butyl acetate, ethylene glycol ether acetate, Propylene glycol n-propyl ether, propylene glycol monomethyl ether acetic acid
Ester, propylene glycol monomethyl ether, DBE (dimethyl succinate, the group of three kinds of environmentally friendly solvents of dimethyl glutarate and hexanedioic acid dimethyl ester
At least one of close) etc..
The preparation method of the carbon series conductive ink comprises the following steps：
1) solvent is mixed with binding agent, until obtaining transparent binding agent mixed liquor；
2) after expanded graphite ball milling, conductive filler, binding agent mixed liquor, curing agent and auxiliary agent are added, continues ball milling, must starch
Material；
3) carbon series conductive ink will be produced after slurries filtration.
In step 2) in, the time of the expanded graphite ball milling can be 0.1~10h, the method for the expanded graphite ball milling
It can be dry ball milling；The time for continuing ball milling can be 0.5~50h, and drum's speed of rotation can be 150~500rpm.
The advantage of the invention is that：
1. utilizing latent curing agent, the electrically conductive ink stability prepared is good, it is easy to preserve.
2. coordinating curing agent using curing accelerator, as little as 80 DEG C insulation 10min of condition of cure belong to low-temperature short-time drying
Type ink, shortens man-hour, reduces energy consumption.
3. shorten ink technique manufacturing cycle.By conventional technique, under one-step method ball milling condition, expanded graphite absorbs molten
Leather hard is presented after agent, grinding efficiency is low.And the present invention uses two-step method ball milling, first carry out dry method independent to expanded graphite
Ball milling, obtains expanded graphite microplate, adds other components and substantially increases grinding efficiency, significantly shorten Ball-milling Time.
Cause ink electric conductivity to decline 4. being directly added into the graphene peeled off and often introducing surfactant, and reduce
Graphene oxide contains a large amount of oxygen-containing functional groups, and defect is more, also results in electric conductivity decline.The stone peeled off with being introduced directly into
Black alkene is compared, and is introduced graphene presoma expanded graphite and be not only simplify the technique peeled off and disperseed, and reduces ink cost, and
The electric conductivity of ink is effectively increased, obtained graphite microchip is peeled off simultaneously during preparing electrically conductive ink or graphene is oxygen-containing
Ratio is extremely low, and defect is few, and electric conductivity is good.
5. obtained graphite microchip or graphene are peeled off during preparing electrically conductive ink simultaneously to carry out resinoid bond
Toughness reinforcing, makes it have good anti-crawl agentdefiection folding endurance, is conducive to the application on flexible material surface.
Brief description of the drawings
Fig. 1 is that the carbon series conductive ink obtained by embodiment 1 prints and gained after baking and curing on mylar PET
The SEM figures of film.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but the invention is not limited in following embodiments.
Embodiment 1：
Ink 1：A kind of carbon series conductive ink, including following components by weight：By expanded graphite and conductive charcoal
Black 20 parts of the bi-component electrically conductive filler constituted respectively by 3 ︰ 1 mass ratio, 15 parts of epoxy resin, 2 parts of curing agent urea, solidification promotees
It is the 0.3% of hardener dose to enter agent DMP-30, is made up of film forming agent, defoamer and thixotropic agent by the ︰ 0.5 of 4 ︰ 1 mass ratio
4 parts of mixed aid, remaining is the mixed solvent being made up of terpinol and ethanol by 3 ︰ 7 mass ratio.Fig. 1 illustrates its ink dry film
Fully contacted between surface conductance particle, particulate is smaller than the normal migration distance of atom (about 10nm), conductive ink film is along outer
Power-up field direction can form continuous conductive path.
Embodiment 2：
Ink 2：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, conductive black
30 parts of the bi-component electrically conductive filler constituted respectively by the ︰ 3 of 5 ︰ 2 mass ratio with CNT, 10 parts of epoxy resin, curing agent methyl
10 parts of tetrabydrophthalic anhydride, DMP-10 and DMP-30 are by 4 ︰ 1 mass ratio composition curing accelerator, curing accelerator consumption
For the 1% of hardener dose, 4 parts of mixed aid being made up of film forming agent, defoamer and thixotropic agent by the ︰ 0.5 of 3 ︰ 1 mass ratio,
Remaining is the mixed solvent being made up of ethyl acetate, Propylene glycol n-propyl ether and DBE by the ︰ 1 of 3 ︰ 1 mass ratio.
Embodiment 3：
Ink 3：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, conductive black
25 parts of the bi-component electrically conductive filler constituted respectively by the ︰ 3 of 2 ︰ 2 mass ratio with CNT, 5 parts of epoxy resin, curing agent 2- second
2 parts of base -4-methylimidazole, benzyl dimethylamine and DMP-30 are by 1 ︰ 1 mass ratio composition curing accelerator, curing accelerator consumption
For the 1% of hardener dose, 2 parts of mixed aid being made up of film forming agent, defoamer and plasticizer by the ︰ 1 of 2 ︰ 1 mass ratio, its
The remaining mixed solvent to be made up of ethyl acetate and DBE by 3 ︰ 2 mass ratio.
Embodiment 4：
Ink 4：A kind of carbon series conductive ink, including following components by weight：By expanded graphite and acetylene black
Divide 15 parts of the bi-component electrically conductive filler constituted by 1 ︰ 1 mass ratio, 3 parts of epoxy resin, 0.5 part of curing agent ethylene diamine, solidification promotees
It is the 1% of hardener dose to enter agent benzyl dimethylamine consumption, and the ︰ 1 of 2 ︰ 1 mass ratio group is pressed by film forming agent, thickener and defoamer
Into 4 parts of mixed aid, remaining is that the mixing being made up of by the ︰ 1 of 2 ︰ 2 mass ratio ethyl acetate, Propylene glycol n-propyl ether and DBE is molten
Agent.
Embodiment 5：
Ink 5：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, conductive black
20 parts of the bi-component electrically conductive filler constituted respectively by the ︰ 3 of 8 ︰ 2 mass ratio with graphene, 6 parts of epoxy resin, curing agent methyl four
6 parts of hydrogen phthalic anhydride, dimethylamino cresols and DMP-30 are by 1 ︰ 1 mass ratio composition curing accelerator, curing accelerator
Consumption is the 1% of hardener dose, the mixed aid 4 being made up of film forming agent, defoamer and thixotropic agent by the ︰ 0.5 of 3 ︰ 1 mass ratio
Part, remaining is DBE solvents.
Embodiment 6：
Ink 6：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, conductive black
5 are pressed respectively：12 parts of the bi-component electrically conductive filler of 1 mass ratio composition, 10 parts of epoxy resin, curing agent 1,3- methylimidazole iodine
2 parts of salt, curing accelerator DMP-10 consumptions are the 3% of hardener dose, by film forming agent, defoamer and thixotropic agent by the ︰'s 1 of 3 ︰ 1
4 parts of the mixed aid of mass ratio composition, remaining is molten for the mixing being made up of butanone, isophorone and DBE by the ︰ 1 of 3 ︰ 1 mass ratio
Agent.
Embodiment 7：
Ink 7：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, graphite and carbon
18 parts of the bi-component electrically conductive filler that nanotube is constituted by the ︰ 1 of 5 ︰ 1 mass ratio respectively, 5 parts of epoxy resin, curing agent 1,3- diformazans
10 parts of base iodonium imidazolide salts, DMP-20 and DMP-30 are by 4 ︰ 1 mass ratio composition curing accelerator, and curing accelerator consumption is solidification
The 1% of agent consumption, 4 parts of mixed aid being made up of film forming agent, defoamer and thixotropic agent by the ︰ 0.5 of 3 ︰ 1 mass ratio, remaining is
The mixed solvent being made up of ethyl acetate, n-butyl acetate and DBE by the ︰ 1 of 3 ︰ 2 mass ratio.
Embodiment 8：
Ink 8：A kind of carbon series conductive ink, including following components by weight：By expanded graphite, conductive black
30 parts of the bi-component electrically conductive filler constituted respectively by the ︰ 3 of 5 ︰ 2 mass ratio with CNT, 10 parts of epoxy resin, curing agent dicyan
10 parts of amine, curing accelerator dimethylamino cresols consumption is the 1% of hardener dose, by film forming agent, stabilizer agent and thixotropic agent
5 parts of the mixed aid constituted by the ︰ 2 of 3 ︰ 1 mass ratio, remaining is by the ︰'s 1 of 1 ︰ 1 by ethyl acetate, Propylene glycol n-propyl ether and DBE
The mixed solvent of mass ratio composition.
Table 1
| Embodiment | Solid content (%) | Thickness (μm) | Square resistance (Ω/) | Fineness (μm) | Adhesive force |
| 1 | 20 | 25 | 5.782 | 5 | 5B |
| 2 | 30 | 25 | 4.498 | 5 | 5B |
| 3 | 25 | 25 | 7.082 | 5 | 5B |
| 4 | 15 | 25 | 23.08 | 5 | 5B |
| 5 | 20 | 25 | 11.28 | 5 | 5B |
| 6 | 12 | 25 | 22.56 | 5 | 5B |
| 7 | 18 | 25 | 18.06 | 5 | 5B |
| 8 | 30 | 25 | 6.112 | 5 | 5B |
Table 1 is the performance parameter using the electrically conductive ink prepared by embodiment 1~8, and condition of cure is 80 DEG C of dryings
10min。
Claims (10)
1. a kind of carbon series conductive ink, it is characterised in that its component is in mass ratio：
Conductive filler 5~40, binding agent 2~20, curing agent 0.1~8, auxiliary agent 0.1~10, solvent 20~80；The conduction is filled out
Material includes component one and component two, and the component one is expanded graphite, the component two be graphene, graphite, conductive carbon fibre,
The mass ratio of at least one of CNT, conductive black, acetylene black, the component one and component two is (0.1~10) ︰ 1.
2. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the binding agent is selected from epoxy resin, acrylic acid
At least one of resin, ternary chlorine vinegar acid resin, polyurethane resin, polyamide.
3. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the curing agent is selected from amine curing agent, imidazoles
At least one of class curing agent, acid anhydride type curing agent；The amine curing agent be selected from urea, ethylenediamine, triethylene tetramine,
At least one of phenylenediamine, polyamide, cdicynanmide.
4. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the imidazole curing agent is selected from 1,3- diformazans
At least one of base iodonium imidazolide salts, 2-ethyl-4-methylimidazole, 2-methylimidazole.
5. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the acid anhydride type curing agent receives enlightening selected from methyl
At least one of gram acid anhydrides, methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride；The curing agent includes
Curing accelerator, the mass percentage content of the curing accelerator is the 0.01%~10% of curing agent；The solidification promotes
Agent is selected from least one of benzyl dimethylamine, dimethylamino cresols, DMP-10, DMP-20, DMP-30.
6. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the auxiliary agent be selected from dispersant, stabilizer, into
At least one of film, coupling agent, plasticizer, defoamer, thickener, levelling agent, thixotropic agent.
7. a kind of carbon series conductive ink as claimed in claim 1, it is characterised in that the solvent be selected from methanol, ethanol, n-butanol,
Isobutanol, terpinol, isopropanol, glycerine, ethyl acetate, cyclohexanone, butanone, isophorone, n-butyl acetate, ethylene glycol ethyl ethers
At least one of ether acetate, Propylene glycol n-propyl ether, propylene glycol methyl ether acetate, propylene glycol monomethyl ether, DBE, the DBE are fourth
The combination of acid dimethyl, three kinds of solvents of dimethyl glutarate and hexanedioic acid dimethyl ester.
8. a kind of preparation method of carbon series conductive ink as claimed in claim 1, it is characterised in that comprise the following steps：
1) solvent is mixed with binding agent, until obtaining transparent binding agent mixed liquor；
2) after expanded graphite ball milling, conductive filler, binding agent mixed liquor, curing agent and auxiliary agent are added, continues ball milling, obtains slurry；
3) carbon series conductive ink will be produced after slurries filtration.
9. a kind of preparation method of carbon series conductive ink as claimed in claim 8, it is characterised in that in step 2) in, the expansion
The time of graphite ball milling is 0.1~10h, and the method for the expanded graphite ball milling is dry ball milling.
10. a kind of preparation method of carbon series conductive ink as claimed in claim 8, it is characterised in that the time of the continuation ball milling
For 0.5~50h, drum's speed of rotation is 150~500rpm.
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| CN201710751355.8A CN107298901A (en) | 2017-08-28 | 2017-08-28 | A kind of carbon series conductive ink |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325627A (en) * | 2017-08-28 | 2017-11-07 | 厦门大学 | Electrically conductive ink low-temperature setting composition and preparation method thereof |
| CN107641376A (en) * | 2017-11-14 | 2018-01-30 | 安徽同利塑胶彩印有限公司 | A kind of printing-ink |
| CN109385145A (en) * | 2018-10-30 | 2019-02-26 | 宁波石墨烯创新中心有限公司 | A kind of organic system electrically conductive ink, preparation method and flexible device |
| CN109456645A (en) * | 2018-10-31 | 2019-03-12 | 华侨大学 | One kind exempting from surfactant graphene composite conductive ink |
| CN109587843A (en) * | 2018-12-12 | 2019-04-05 | 杭州华暖科技有限公司 | A kind of electric heating electric hot plate and preparation method thereof |
| CN110093645A (en) * | 2019-05-31 | 2019-08-06 | 厦门大学 | Plastic electroplating method |
| CN110467846A (en) * | 2019-08-21 | 2019-11-19 | 厦门大学 | A kind of preparation method of oiliness electric heating conversion ink and prepared ink |
| CN110628264A (en) * | 2019-08-21 | 2019-12-31 | 厦门大学 | Preparation method of graphene far-infrared additive and far-infrared slurry |
| CN111326274A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Modified graphene composite slurry with high dispersion stability and preparation method thereof |
| CN111410871A (en) * | 2020-03-06 | 2020-07-14 | 南昌欧菲生物识别技术有限公司 | Conductive ink, display module and electronic equipment |
| CN111690296A (en) * | 2020-07-22 | 2020-09-22 | 广东一纳科技有限公司 | Composite carbon material ink and preparation method and application thereof |
| WO2021031464A1 (en) * | 2019-08-21 | 2021-02-25 | 厦门大学 | Method for preparing graphene far infrared additive and far infrared paste |
| CN113571232A (en) * | 2021-07-20 | 2021-10-29 | 苏州英纳电子材料有限公司 | Bottom black carbon slurry based on printed metal grid conductive film and preparation method thereof |
| CN116120784A (en) * | 2022-12-28 | 2023-05-16 | 厦门大学 | Conductive ink and preparation method thereof, plastic material and preparation method thereof, and electroplated plastic |
| CN116120785A (en) * | 2022-12-28 | 2023-05-16 | 厦门大学 | Conductive ink and preparation method thereof, plastic material and preparation method thereof, and electroplated plastic |
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| CN107325627A (en) * | 2017-08-28 | 2017-11-07 | 厦门大学 | Electrically conductive ink low-temperature setting composition and preparation method thereof |
| CN107641376A (en) * | 2017-11-14 | 2018-01-30 | 安徽同利塑胶彩印有限公司 | A kind of printing-ink |
| CN109385145A (en) * | 2018-10-30 | 2019-02-26 | 宁波石墨烯创新中心有限公司 | A kind of organic system electrically conductive ink, preparation method and flexible device |
| CN109456645A (en) * | 2018-10-31 | 2019-03-12 | 华侨大学 | One kind exempting from surfactant graphene composite conductive ink |
| CN109456645B (en) * | 2018-10-31 | 2021-10-01 | 华侨大学 | Surfactant-free graphene composite conductive ink |
| CN109587843A (en) * | 2018-12-12 | 2019-04-05 | 杭州华暖科技有限公司 | A kind of electric heating electric hot plate and preparation method thereof |
| CN111326274A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Modified graphene composite slurry with high dispersion stability and preparation method thereof |
| CN111326274B (en) * | 2018-12-13 | 2022-01-28 | 山东欧铂新材料有限公司 | Modified graphene composite slurry with high dispersion stability and preparation method thereof |
| CN110093645A (en) * | 2019-05-31 | 2019-08-06 | 厦门大学 | Plastic electroplating method |
| CN110628264A (en) * | 2019-08-21 | 2019-12-31 | 厦门大学 | Preparation method of graphene far-infrared additive and far-infrared slurry |
| CN110467846A (en) * | 2019-08-21 | 2019-11-19 | 厦门大学 | A kind of preparation method of oiliness electric heating conversion ink and prepared ink |
| WO2021031464A1 (en) * | 2019-08-21 | 2021-02-25 | 厦门大学 | Method for preparing graphene far infrared additive and far infrared paste |
| CN111410871A (en) * | 2020-03-06 | 2020-07-14 | 南昌欧菲生物识别技术有限公司 | Conductive ink, display module and electronic equipment |
| WO2021175100A1 (en) * | 2020-03-06 | 2021-09-10 | 欧菲光集团股份有限公司 | Electrically-conductive ink, display module, and electronic apparatus |
| CN111690296A (en) * | 2020-07-22 | 2020-09-22 | 广东一纳科技有限公司 | Composite carbon material ink and preparation method and application thereof |
| CN113571232A (en) * | 2021-07-20 | 2021-10-29 | 苏州英纳电子材料有限公司 | Bottom black carbon slurry based on printed metal grid conductive film and preparation method thereof |
| CN116120784A (en) * | 2022-12-28 | 2023-05-16 | 厦门大学 | Conductive ink and preparation method thereof, plastic material and preparation method thereof, and electroplated plastic |
| CN116120785A (en) * | 2022-12-28 | 2023-05-16 | 厦门大学 | Conductive ink and preparation method thereof, plastic material and preparation method thereof, and electroplated plastic |
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Application publication date: 20171027 |