CN110634590A - Wear-resistant conductive paste and preparation method thereof - Google Patents
Wear-resistant conductive paste and preparation method thereof Download PDFInfo
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- CN110634590A CN110634590A CN201910842240.9A CN201910842240A CN110634590A CN 110634590 A CN110634590 A CN 110634590A CN 201910842240 A CN201910842240 A CN 201910842240A CN 110634590 A CN110634590 A CN 110634590A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a wear-resistant conductive paste and a preparation method thereof, wherein the conductive paste comprises, by weight, 4-10 parts of matrix resin, 5-30 parts of ester solvent, 0.6-1.7 parts of adhesion promoter, 0.5-2 parts of thickener, 0.2-0.8 part of defoamer, 1.5-2.8 parts of anti-settling additive, 0.5-1.8 parts of curing catalyst, 10-20 parts of wear-resistant powder and 40-70 parts of conductive powder. The wear-resistant silver paste prepared by the invention has higher viscosity due to the addition of the thickening agent, the adhesive force of the paste is improved, bubbles generated in the production process of the paste can be eliminated by adding the defoaming agent, the smoothness of the finally prepared silver paste is improved, and the wear resistance of the finally prepared silver paste is improved.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to wear-resistant conductive paste and a preparation method thereof.
Background
The conductive paste is widely applied to electronic information products due to good physical properties of the conductive paste, and higher requirements are put forward on the performance of the conductive paste along with the development of lighter, thinner, more powerful functionality and more environment-friendly electronic products. The low-temperature halogen-free conductive silver paste is widely applied to aspects such as film switches, capacitance electrodes, touch screens and the like due to excellent electrical conductivity, thermal conductivity and practicability. The low-temperature conductive silver paste is uniform paste prepared by stirring and dispersing conductive silver powder serving as a conductive filler, high polymer resin, a solvent, a curing agent, an auxiliary agent and the like. After the conductive silver paste is coated on a base material, the base material is dried in a low-temperature environment (generally lower than 160 ℃), and after the solvent is released, the resin and the curing agent gradually react and cure to finally form a compact conductive film layer.
In the electronic industry, in order to meet the requirements of high strength and high mechanical properties of products, the conductive film layer of the low-temperature conductive silver paste after curing generally has mechanical requirements (film layer hardness, film layer and substrate adhesion, and the like). The conductive silver powder is metal powder and has relatively high hardness, but the hardness of high polymers such as resin is generally poor. When the high hardness requirement is met by increasing the filling amount of the silver powder, the silver powder cannot be fully and effectively coated by a relatively small amount of resin, so that the silver powder on the surface layer is not firmly adsorbed and falls off.
The wear-resistant conductive paste is a novel conductive material which combines the wear resistance and the conductivity of the conductive paste, and can be used for products with high requirements on the wear resistance of the paste.
Disclosure of Invention
The embodiment of the invention provides wear-resistant conductive paste and a preparation method thereof.
In order to solve the above technical problem, an embodiment of the first aspect of the present invention provides a wear-resistant conductive paste, including, by weight: 4-10 parts of matrix resin, 5-30 parts of ester solvent, 0.6-1.7 parts of adhesion promoter, 0.5-2 parts of thickening agent, 0.2-0.8 part of defoaming agent, 1.5-2.8 parts of anti-settling additive, 0.5-1.8 parts of curing catalyst, 10-20 parts of wear-resistant powder and 40-70 parts of conductive powder.
Further, the matrix resin is selected from polyketone resin or acrylic resin.
Further, the ester solvent is selected from DBE, diethyl adipate, butyl acetate, diethylene glycol ethyl ether acetate, ethylene glycol butyl ether, dimethyl glutarate, dimethyl adipate or a plurality of DBE, diethyl adipate, butyl acetate, diethylene glycol ethyl ether acetate, ethylene glycol butyl ether, dimethyl glutarate and dimethyl adipate.
Further, the thickening agent is selected from carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium polyacrylate, organic bentonite, polyacrylamide or xanthan gum.
Further, the antifoaming agent is selected from BYK333 or TEGO FOAMEX 810.
Further, the anti-settling auxiliary agent is selected from polyethylene wax, nano carbon black particles or fumed silica.
Further, the curing catalyst is selected from isocyanate, dicyandiamide, organic synthetic amines or platinum catalysts.
Further, the wear-resistant powder is selected from nickel powder, copper powder or aluminum powder.
Further, the conductive powder is selected from one or more of spherical silver powder, flake silver powder, dendritic silver powder or rod silver powder.
The embodiment of the second aspect of the present invention provides a preparation method of a wear-resistant conductive paste, which adopts the conductive paste formulation according to the embodiment of the first aspect, and includes the following steps:
(1) preparing a high molecular resin carrier, weighing a base resin according to the formula amount, mixing the base resin and a solvent, completely dissolving at 60-90 ℃, filtering and removing impurities from the high molecular resin carrier on a 200-400-mesh sieve to obtain the high molecular resin carrier, and detecting the viscosity value of the high molecular resin carrier, wherein the required value is 1000-4000 cps;
(2) preparing conductive slurry, namely weighing an adhesion promoter, a thickening agent, a defoaming agent, an anti-settling auxiliary agent, wear-resistant powder, conductive powder, a curing catalyst and 20-40 wt% of the polymer resin carrier prepared in the step (1) according to the formula, mixing the raw materials in a mixer for 1h to obtain premix, uniformly mixing the premix, the wear-resistant filler and silver powder in a certain proportion, controlling the temperature to be in the range of-10-5 ℃, and performing high-speed shearing, grinding and dispersing in a grinder to obtain the conductive slurry;
(3) and (3) post-processing the conductive paste, namely filtering the conductive paste obtained in the step (2) through a 200-ion 800-mesh screen to remove impurities or disperse uneven larger particles in the paste, then placing the filtered conductive paste in a vacuum defoaming machine, vacuumizing to obtain the conductive paste, and detecting the viscosity value of the conductive paste, wherein the required value is 30000-40000 cps.
The invention achieves the following beneficial effects: except for basic preparations, the thickening agent and the defoaming agent are added into the formula of the conductive paste, secondary defoaming is performed in the preparation method, the viscosity of the silver paste is increased, and meanwhile, a better defoaming effect is achieved, so that the excellent friction resistance of the conductive paste is realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of a method for preparing a wear-resistant conductive paste according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the preparation method of the conductive paste has the following steps:
weighing a certain proportion of matrix resin and an ester solvent according to the total mass percentage of the formula in the step (1) as materials for preparing a high polymer resin carrier, preferably weighing 8% of matrix resin and 22% of ester solvent to mix, completely dissolving at 90 ℃ to obtain the high polymer resin carrier, filtering and removing impurities from the obtained high polymer resin carrier on a 200-mesh screen to obtain the final high polymer resin carrier, and further detecting the viscosity value of the high polymer resin carrier, wherein the viscosity value of the high polymer resin carrier needs to meet 1000-4000cps, and products beyond the range do not enter the next procedure.
It is understood that the minimum fusion temperature of the matrix resin and the ester solvent can be set at 60 ℃, and the larger the mesh number of the screen, the less the impurities contained in the polymer resin carrier, but the mesh number of the screen as the first step can be set within the range of 200-400 mesh considering the cost and the requirements of the finally prepared silver paste. And other large-particle impurities cannot enter the subsequent preparation process, so that a screen with a large number of meshes is not required to be selected for filtering in the primary filtering of the first process, and the screen with the large number of meshes is adopted again for secondary filtering to ensure that the impurity content does not exceed the standard after the wear-resistant silver paste is finally prepared.
And (2) weighing each additive and the final polymer resin carrier prepared in the step (1) according to the formula amount, and fully mixing the weighed raw materials in a mixer to obtain a premix, wherein an adhesion promoter in the additive can be selected from a silane coupling agent, a titanate coupling agent or an aluminate coupling agent. Further, the premix, the nickel powder and the silver powder are subjected to high-speed shearing, grinding and dispersion in a grinding machine, the temperature is controlled within the range of-10 ℃ to 5 ℃, and the resin and the curing agent are prevented from reacting in the grinding process to obtain the conductive slurry. The temperature control is particularly important, the optimal temperature range obtained through multiple times of test data analysis is-10-5 ℃, and the temperature can be usually maintained at about 0 ℃.
The nickel powder is a wear-resistant powder, the nickel powder is used as a skeleton of the wear-resistant silver paste to increase the hardness of the silver paste, and the nickel powder has certain conductivity and can properly reduce the content of the conductive powder.
And (3) filtering the obtained conductive paste through a 800-mesh screen to remove impurities or large non-uniform dispersed particles in the paste, then placing the filtered conductive silver paste in a vacuum defoaming machine, vacuumizing to obtain the conductive paste, wherein the viscosity value of the detector is 30000-40000cps, and the product beyond the range is not subjected to the next process, namely the detection process of the product is not performed. Wherein, because of adding the thickening agent, the wear-resisting silver paste can reach the viscosity value of higher requirement.
It should be noted that, because the mesh number of the screen in step 1 is smaller, the polymer resin carrier contains a part of impurities, and after all the preparation processes are completed, the finally prepared wear-resistant silver paste can be subjected to fine filtration by using the screen with a larger mesh number, so that the prepared wear-resistant silver paste is ensured to contain fewer impurities.
In the application, the following detection method can be adopted to detect the properties of the prepared wear-resistant silver paste:
(1) and (3) wear resistance test: paper tape rubbing and rubber rubbing;
(2) measuring the volume resistivity; a resistivity tester;
(3) high temperature and high humidity experiment: storing at 85 deg.C and 85% humidity for 1500 hr;
(4) salt spray experiment: spraying with 5% +/-1% NaCl saline for 72h under sealed condition of 35 + -2 deg.C and environment humidity greater than 80% and pH value of 6.5-7.2.
In the preferred embodiment of the present application, the formulation ratio of each preparation in the formulation can be several as shown in table 1.
Table 1 shows the composition ratios of the components in the examples
The conductive paste prepared in the above example was tested: paper tape rubbing (175gf rolling rubbing, standard 200 cycles) and rubber rubbing (500gf rubber back and forth rubbing 100 cycles), volume resistivity < 1X 10-5Omega cm, does not oxidize after being stored for 1500 hours in a high-temperature and high-humidity environment, has good appearance in a salt spray experiment, has the resistance change of less than 10 percent and has the adhesive force of grade 5B.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The wear-resistant conductive paste is characterized by comprising, by weight, 4-10 parts of matrix resin, 5-30 parts of an ester solvent, 0.6-1.7 parts of an adhesion promoter, 0.5-2 parts of a thickening agent, 0.2-0.8 part of a defoaming agent, 1.5-2.8 parts of an anti-settling auxiliary agent, 0.5-1.8 parts of a curing catalyst, 10-20 parts of wear-resistant powder and 40-70 parts of conductive powder.
2. The conductive paste of claim 1, wherein the matrix resin is selected from a polyketone resin or an acrylic resin.
3. The conductive paste of claim 1, wherein the ester solvent is selected from DBE, diethyl adipate, butyl acetate, diethylene glycol ethyl ether acetate, ethylene glycol butyl ether, dimethyl glutarate, dimethyl adipate, or a plurality thereof.
4. The conductive paste of claim 1, wherein the thickener is selected from the group consisting of carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium polyacrylate, organic bentonite, polyacrylamide, and xanthan gum.
5. The conductive paste of claim 1, wherein the defoamer is selected from BYK333 or TEGO FOAMEX 810.
6. The conductive paste of claim 1, wherein the anti-settling additive is selected from polyethylene wax, nano carbon black particles, or fumed silica.
7. The conductive paste of claim 1, wherein the curing catalyst is selected from isocyanate, dicyandiamide, organic synthetic amines or platinum-gold catalyst.
8. The conductive paste of claim 1, wherein the wear-resistant powder is selected from nickel powder, copper powder, and aluminum powder.
9. The conductive paste of claim 1, wherein the conductive powder is selected from one or more of spherical silver powder, flake silver powder, dendritic silver powder, and rod silver powder.
10. A method for preparing a wear-resistant conductive paste, based on the conductive paste formulation of any one of claims 1 to 9, comprising the steps of:
(1) preparing a high molecular resin carrier, weighing a base resin according to the formula amount, mixing the base resin and a solvent, completely dissolving at 60-90 ℃, filtering and removing impurities from the high molecular resin carrier on a 200-400-mesh sieve to obtain the high molecular resin carrier, and detecting the viscosity value of the high molecular resin carrier, wherein the required value is 1000-4000 cps;
(2) preparing conductive slurry, namely weighing an adhesion promoter, a thickening agent, a defoaming agent, an anti-settling auxiliary agent, wear-resistant powder, conductive powder, a curing catalyst and 20-40 wt% of the polymer resin carrier prepared in the step (1) according to the formula, mixing the raw materials in a mixer for 1h to obtain premix, uniformly mixing the premix, the wear-resistant filler and silver powder in a certain proportion, controlling the temperature to be in the range of-10-5 ℃, and performing high-speed shearing, grinding and dispersing in a grinder to obtain the conductive slurry;
(3) and (3) post-processing the conductive paste, namely filtering the conductive paste obtained in the step (2) through a 200-ion 800-mesh screen to remove impurities or disperse uneven larger particles in the paste, then placing the filtered conductive paste in a vacuum defoaming machine, vacuumizing to obtain the conductive paste, and detecting the viscosity value of the conductive paste, wherein the required value is 30000-40000 cps.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112466509A (en) * | 2020-11-20 | 2021-03-09 | 无锡晶睿光电新材料有限公司 | Low-temperature high-wear-resistance conductive silver paste and preparation method thereof |
| CN113192663A (en) * | 2021-04-25 | 2021-07-30 | 北京梦之墨科技有限公司 | Enhanced conductive paste and electronic device |
| CN113436781A (en) * | 2021-07-27 | 2021-09-24 | 北京中科纳通电子技术有限公司 | Wear-resistant conductive paste and preparation method thereof |
| CN115975323A (en) * | 2022-12-02 | 2023-04-18 | 广州市儒兴科技股份有限公司 | Organic carrier for conductive paste and preparation method thereof |
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| CN101359564A (en) * | 2008-09-16 | 2009-02-04 | 彩虹集团公司 | Anti-Ag diffusion photosensitive and conductive pulp and method for preparing same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112466509A (en) * | 2020-11-20 | 2021-03-09 | 无锡晶睿光电新材料有限公司 | Low-temperature high-wear-resistance conductive silver paste and preparation method thereof |
| CN113192663A (en) * | 2021-04-25 | 2021-07-30 | 北京梦之墨科技有限公司 | Enhanced conductive paste and electronic device |
| CN113436781A (en) * | 2021-07-27 | 2021-09-24 | 北京中科纳通电子技术有限公司 | Wear-resistant conductive paste and preparation method thereof |
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| CN115975323A (en) * | 2022-12-02 | 2023-04-18 | 广州市儒兴科技股份有限公司 | Organic carrier for conductive paste and preparation method thereof |
| CN115975323B (en) * | 2022-12-02 | 2023-12-12 | 广州市儒兴科技股份有限公司 | Organic carrier for conductive paste and preparation method thereof |
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Application publication date: 20191231 |