CN110591453A - Low-temperature curing conductive ink with oxidation resistance and low corrosion resistance - Google Patents
Low-temperature curing conductive ink with oxidation resistance and low corrosion resistance Download PDFInfo
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- CN110591453A CN110591453A CN201911009136.8A CN201911009136A CN110591453A CN 110591453 A CN110591453 A CN 110591453A CN 201911009136 A CN201911009136 A CN 201911009136A CN 110591453 A CN110591453 A CN 110591453A
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- 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
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
The invention discloses an antioxidant low-corrosion conductive ink capable of being cured at low temperature, which comprises, by weight, 30-75 parts of a resin intermediate, 4-25 parts of a solvent, 0.5-5 parts of an antioxidant, 10-50 parts of silver powder and 0.5-5 parts of an auxiliary agent. The resin is hydroxyl or carboxyl modified ternary vinyl chloride-vinyl acetate copolymer resin with molecular weight of 15000-65000 and K of 35-60. The solvent is one or more selected from diethylene glycol butyl ether acetate, diethylene glycol butyl ether, ethylene glycol butyl ether acetate, ethylene glycol butyl ether, 1, 4-butanediol, triethylene glycol butyl ether, tripropylene glycol, diethylene glycol, tripropylene glycol butyl ether, 3-methoxy-3-methyl-1-butanol and dipropylene glycol methyl ether, and the resin intermediate is resin after solvent dilution. The invention effectively changes the gradual yellowing phenomenon of the surface of the conductive ink paint film, can also prevent the bottom biting defect of the conductive ink on plastic films such as PVC, PC, ABS, PMMA and other substrates, and effectively improves the product quality.
Description
Technical Field
The invention relates to a conductive ink, in particular to an antioxidant low-corrosion low-temperature curing conductive ink.
Background
The low-temperature cured conductive ink is widely applied to the fields of electronic components such as display screens, membrane switches, flexible circuits and the like, and makes the lightening, thinning and intelligentization of electronic products possible. However, with the development of electronic products such as foldable mobile phones, curved televisions and the like which are widely popularized in the market in recent years, higher requirements are placed on the performance of flexible screens and flexible circuits, and further higher performance requirements are placed on conductive ink which plays a key role in such electronic components.
The traditional conductive ink or conductive silver paste is usually printed on the surface of aging-resistant and corrosion-resistant substrates such as PET (polyethylene terephthalate plastic), silicone, PP (polypropylene plastic), PE (polyethylene plastic), PI (polyimide plastic), ITO (indium tin oxide), glass, and the like, so that the raw materials and solvents used by the conductive ink are not harsh, and the conductive ink is sealed by insulating glue or an insulating film after the surface of the substrates is cured, thereby isolating the contact between the ink and air and preventing the cured ink from being oxidized.
However, with the advance of science and technology, in order to realize the flexibility of electronic components, conductive ink needs to be printed on film substrates which are not resistant to solvent corrosion, such as PC (polycarbonate plastic), PVC (polyvinyl chloride plastic), ABS (engineering plastic), PMMA (acrylic plastic), and the like, so that the substrates are easily swelled and deformed by corrosive solvents in the production process, and the conventional conductive ink or conductive silver paste generally needs to use ketone and ester solvents as diluents to adjust the viscosity, so as to facilitate the construction such as printing and coating, and these solvents include cyclohexanone, isophorone, DBE, ethylene glycol diacetate, and the like, which not only has unpleasant odor, but also easily causes the corrosion of the substrates, and the phenomenon of 'bottom biting' occurs. In addition, in order to ensure high flexibility of the electronic element, the insulating glue or the insulating film structure is gradually cancelled, so that the membrane switch or the flexible circuit needs to be exposed in the air, the conductive ink is easily oxidized by the outside air and soaked by sweat of a human body, yellowing and the like are caused, and the service life is shortened.
Disclosure of Invention
The invention provides an antioxidant low-corrosion low-temperature curing conductive ink, which at least solves the problem that the conductive ink in the prior art is easy to corrode plastics.
The invention provides an antioxidant low-corrosion low-temperature curing conductive ink which is prepared from the following raw materials in parts by weight: 30-75 parts of resin intermediate, 4-25 parts of solvent, 0.5-5 parts of antioxidant, 10-50 parts of silver powder and 0.5-5 parts of auxiliary agent, wherein the resin intermediate consists of 60-95% of resin and 5-40% of solvent, and the solvent is low-corrosion solvent.
Further, the average polymerization degree of the resin is 35 to 60.
Still further, the resin is selected from one or two of hydroxyl modified ternary vinyl chloride-vinyl acetate copolymer and carboxyl modified ternary vinyl chloride-vinyl acetate copolymer, and the molecular weight of the resin is between 15000 and 65000.
Further, the solvent is selected from one or more of diethylene glycol butyl ether acetate, diethylene glycol butyl ether, ethylene glycol butyl ether acetate, ethylene glycol butyl ether, 1, 4-butanediol, triethylene glycol butyl ether, tripropylene glycol, diethylene glycol, tripropylene glycol butyl ether, 3-methoxy-3-methyl-1-butanol and dipropylene glycol methyl ether.
Further, the antioxidant is prepared from a heat-resistant oxidant and an ultraviolet absorber according to the ratio of (0.1-10): (0.1-10) by weight;
the heat-resistant oxidant is selected from one or more of pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), tris [2, 4-di-tert-butylphenyl ] phosphite, N '-bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, thiodiethylbis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], and didodecyl thiodipropionate;
the ultraviolet absorbent is selected from one or more of 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-5 ' -tert-octylphenyl) benzotriazole, 2-hydroxy-4-n-octyloxybenzophenone, 2- (2' -hydroxy-5 ' -methylphenyl) benzotriazole, 2' - (2' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole, and bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate.
Further, the silver powder is antioxidant micron-sized flaky silver powder, and the average particle size of the silver powder is 2.0-12.0 microns.
Further, the silver powder has a bulk density of 0.2 to 0.9g/cm3The tap density is 1.0 to 4.0g/cm3
Further, the auxiliary agent is selected from one or more of a defoaming agent, an adhesion promoter, a dispersing agent and a leveling agent.
The invention also discloses a preparation method of the conductive ink, which comprises the following steps:
step 1: mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 150-mesh and 250-mesh filter screen, and packaging to obtain the final product.
Further, in the step 1, the resin intermediate needs to be preheated to 30-45 ℃ before mixing, and is uniformly dispersed in a high-speed shear disperser according to the conditions of 500-1200 r/min.
Compared with the prior art, the conductive ink disclosed by the invention solves the problem that the conductive ink has higher corrosion capability on substrates such as PC (polycarbonate plastic), PVC (polyvinyl chloride plastic), ABS (engineering plastic), PMMA (acrylic plastic) and the like, ensures that the conductive ink has the advantages of low corrosion, sweat resistance, bending resistance, oxidation resistance and low yellowing while maintaining excellent conductivity.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example one
The conductive ink provided by the embodiment of the invention is composed of the following raw materials in parts by weight: 45 parts of a resin intermediate, 4 parts of ethylene glycol butyl ether acetate, 5 parts of ethylene glycol butyl ether, 1 part of tris [ 2.4-di-tert-butylphenyl ] phosphite, 0.5 part of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 0.5 part of a high molecular weight polyester adhesion promoter, 43 parts of silver powder, 0.5 part of a dispersant, and 0.5 part of a defoamer, wherein the resin intermediate is composed of 80 parts of a hydroxyl-modified trichloroacetic resin and 20 parts of ethylene glycol butyl ether.
The embodiment of the invention provides a method for manufacturing conductive ink, which comprises the following steps:
step 1: mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 230 mesh sieve, packaging to obtain final product, and storing at 5-20 deg.C.
Example two
The second conductive ink of the embodiment of the invention is composed of the following raw materials in parts by weight: 55 parts of a resin intermediate, 10 parts of a solvent, 1 part of tris [2, 4-di-tert-butylphenyl ] phosphite, 0.5 part of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 0.5 part of a high-molecular-weight polyester adhesion promoter, 50 parts of silver powder, 0.5 part of a dispersant, and 0.5 part of a defoamer, wherein the resin intermediate is composed of 60 parts by weight of a carboxyl-modified trichloroacetic resin and 40 parts by weight of ethylene glycol butyl ether.
The second method for manufacturing the conductive ink comprises the following steps:
step 1: mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 230 mesh sieve, packaging to obtain final product, and storing at 5-20 deg.C.
EXAMPLE III
The conductive ink of the embodiment of the invention is composed of the following raw materials in parts by weight: 75 parts of a resin intermediate, 25 parts of a solvent, 1 part of tris [2, 4-di-tert-butylphenyl ] phosphite, 0.5 part of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 0.5 part of a high molecular weight polyester adhesion promoter, 20 parts of silver powder, 0.5 part of a dispersant, and 0.5 part of a defoamer, wherein the resin intermediate is composed of 40 parts by weight of a hydroxy-modified trichloroacetic resin, 40 parts by weight of a carboxy-modified trichloroacetic resin, and 20 parts by weight of ethylene glycol butyl ether.
The preparation method of the conductive ink comprises the following steps:
step 1: preheating the resin intermediate to 30-45 ℃, uniformly dispersing the resin intermediate in a high-speed shearing dispersion machine according to the condition of 500-1200r/min, mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 230 mesh sieve, packaging to obtain final product, and storing at 5-20 deg.C.
Comparative example
The conductive ink of the comparative example consists of the following raw materials in parts by weight: 45 parts of resin intermediate, 4 parts of ethylene glycol diacetate, 5 parts of DBE, 0.5 part of high molecular weight polyester adhesion promoter, 43 parts of silver powder, 0.5 part of dispersant and 0.5 part of defoamer, wherein the resin intermediate consists of 80 parts of hydroxyl modified ternary vinyl chloride-vinyl acetate resin and 20 parts of ethylene glycol butyl ether.
The preparation method of the conductive ink of the comparative example comprises the following steps:
step 1: mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 230 mesh sieve, packaging to obtain final product, and storing at 5-20 deg.C.
The conductive inks prepared in the first, second and third examples of the present invention and the comparative example were subjected to performance tests, and the test results are shown in the first and second tables.
TABLE I basic Performance index of conductive inks of examples one, two, three and comparative examples of the present invention
TABLE II weather resistance test of the first, second and third inventive examples and the comparative example
According to the embodiment of the invention, the alcohols, ethers and alcohol ether solvents with low corrosion to the substrate are used as the diluent, so that the deformation of non-corrosion-resistant substrates such as PC, PVC and the like is effectively avoided. Meanwhile, the embodiment of the invention selects the heat-resistant oxidant to prevent the conductive ink from being oxidized and yellowed due to heating in the curing process. In addition, the ultraviolet absorbent of the embodiment of the invention effectively prevents the silver paste from oxidative yellowing caused by the irradiation of indoor or outdoor ultraviolet rays on the cured conductive ink, and the service life of the conductive silver paste is prolonged.
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that the modifications and equivalents of the specific embodiments of the present invention can be made by those skilled in the art after reading the present specification, but these modifications and variations do not depart from the scope of the claims of the present application.
Claims (10)
1. The low-temperature curing conductive ink with the oxidation resistance and the low corrosion resistance is characterized by comprising the following raw materials in parts by weight: 30-75 parts of resin intermediate, 4-25 parts of solvent, 0.5-5 parts of antioxidant, 10-50 parts of silver powder and 0.5-5 parts of auxiliary agent, wherein the resin intermediate consists of 60-95% of resin and 5-40% of solvent, and the solvent is low-corrosion solvent.
2. The low temperature curable conductive ink according to claim 1, wherein the resin has an average degree of polymerization of 35 to 60.
3. The low-temperature-curable conductive ink according to claim 2, wherein the resin is one or two selected from hydroxyl-modified trichloro-vinyl acetate terpolymer and carboxyl-modified trichloro-vinyl acetate terpolymer, and the molecular weight of the resin is 15000 to 65000.
4. The low temperature curable conductive ink according to claim 1, wherein the solvent is selected from one or more of diethylene glycol butyl ether acetate, diethylene glycol butyl ether, ethylene glycol butyl ether acetate, ethylene glycol butyl ether, 1, 4-butanediol, triethylene glycol butyl ether, tripropylene glycol, diethylene glycol, tripropylene glycol butyl ether, 3-methoxy-3-methyl-1-butanol, and dipropylene glycol methyl ether.
5. The low-temperature curable conductive ink according to claim 1, wherein the antioxidant is prepared from a thermal oxidant resistant, ultraviolet absorber in a ratio of (0.1-10): (0.1-10) by weight;
the heat-resistant oxidant is selected from one or more of pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), tris [2, 4-di-tert-butylphenyl ] phosphite, N '-bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, thiodiethylbis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], and didodecyl thiodipropionate;
the ultraviolet absorbent is selected from one or more of 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-5 ' -tert-octylphenyl) benzotriazole, 2-hydroxy-4-n-octyloxybenzophenone, 2- (2' -hydroxy-5 ' -methylphenyl) benzotriazole, 2' - (2' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole, and bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate.
6. The low-temperature curing conductive ink according to claim 1, wherein the silver powder is an oxidation-resistant micron-sized plate-like silver powder, and the average particle size of the silver powder is 2.0 to 12.0 μm.
7. The low-temperature-curable conductive ink according to claim 6, wherein the silver powder has a bulk density of 0.2 to 0.9g/cm3The tap density is 1.0 to 4.0g/cm3。
8. The low-temperature-curing conductive ink as claimed in claim 1, wherein the auxiliary agent is one or more selected from a defoaming agent, an adhesion promoter, a dispersing agent and a leveling agent.
9. A method of making the conductive ink of any one of claims 1-8, comprising the steps of:
step 1: mixing the resin intermediate, the solvent, the antioxidant, the silver powder and the auxiliary agent according to a set proportioning relation, and preheating to 30-45 ℃;
step 2: placing the mixture obtained in the step 1 in a high-speed shearing dispersion machine, uniformly dispersing under the condition of 500-1200r/min, and fully grinding on a three-roll grinder until the particle size is less than 7 mu m;
and step 3: filtering with 150-mesh and 250-mesh filter screen, and packaging to obtain the final product.
10. The method for preparing the conductive ink as claimed in claim 9, wherein the resin intermediate is preheated to 30-45 ℃ before mixing in step 1, and is uniformly dispersed in a high-speed shear disperser at a speed of 500-1200 r/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911009136.8A CN110591453A (en) | 2019-10-23 | 2019-10-23 | Low-temperature curing conductive ink with oxidation resistance and low corrosion resistance |
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| CN201911009136.8A CN110591453A (en) | 2019-10-23 | 2019-10-23 | Low-temperature curing conductive ink with oxidation resistance and low corrosion resistance |
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| CN112271013A (en) * | 2020-10-29 | 2021-01-26 | 无锡晶睿光电新材料有限公司 | Anti-oxidation low-temperature conductive silver paste and preparation method thereof |
| CN112735628A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste and preparation method thereof |
| CN112735629A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste with low silver content and preparation method thereof |
| CN112898821A (en) * | 2021-02-04 | 2021-06-04 | 天津海顺印业包装有限公司 | Low-cost silver scraping and ink printing method for silver scraping card |
| CN114709007A (en) * | 2022-05-07 | 2022-07-05 | 湖南省国银新材料有限公司 | Low-temperature quick-drying silver paste for conductive film and preparation method thereof |
| CN117457260A (en) * | 2023-12-26 | 2024-01-26 | 深圳市绚图新材科技有限公司 | Novel conductive carbon black-modified graphene composite slurry and preparation method thereof |
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Application publication date: 20191220 |