CN112271013A - Anti-oxidation low-temperature conductive silver paste and preparation method thereof - Google Patents
Anti-oxidation low-temperature conductive silver paste and preparation method thereof Download PDFInfo
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- CN112271013A CN112271013A CN202011183957.6A CN202011183957A CN112271013A CN 112271013 A CN112271013 A CN 112271013A CN 202011183957 A CN202011183957 A CN 202011183957A CN 112271013 A CN112271013 A CN 112271013A
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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 relates to an antioxidant low-temperature conductive silver paste and a preparation method thereof, wherein the raw materials comprise the following components in percentage by weight: 6-8% of high molecular resin; 50-60% of metal silver powder; 0.5 to 1.0 percent of curing agent; 0.5 to 1.0 percent of antioxidant auxiliary agent; 2 to 10 percent of thickening agent; 30-40% of a solvent; weighing the polymer resin and the solvent, pouring the polymer resin and the solvent into a dissolving kettle, stirring the mixture until the mixture is transparent, and filtering the mixture by using 300-mesh and 400-mesh gauze to obtain a carrier; weighing the metal silver powder, the curing agent, the antioxidant auxiliary agent and the thickening agent, and placing the metal silver powder, the curing agent, the antioxidant auxiliary agent and the thickening agent into a high-speed centrifugal dispersion machine for high-speed dispersion to obtain uniform slurry; and grinding the slurry in a three-high mill to prepare the antioxidant low-temperature conductive silver paste. Compared with the prior art, the low-temperature conductive silver paste prepared by the invention has the advantages of conductivity and adhesive force of the existing silver paste, excellent oxidation resistance, extremely strong acid-base resistance in high-temperature and high-humidity environments and long service life.
Description
Technical Field
The invention belongs to the technical field of conductive silver paste preparation, and particularly relates to an antioxidant low-temperature conductive silver paste and a preparation method thereof.
Background of the invention
With the development of electronic technology and thin film circuits, the usage amount of conductive silver paste rises year by year, the market demand is very large, and the application of the conductive silver paste is more and more wide, and the conductive silver paste is gradually applied to the fields of notebook keyboards, thin film switches, household appliance control panels, glucometers and the like. The low-temperature conductive silver paste is generally printed on the surface of a substrate by a screen printing technology according to a designed printed circuit, and is subjected to low-temperature heating and baking treatment to enable the silver paste to be attached to the surface of the substrate to form a conductive silver line layer. As the application field of the conductive silver paste is wider and wider, the conductive circuit can be exposed to the environment such as damp heat and the like, so that high technical requirements on the oxidation resistance, acid and alkali resistance, wear resistance, adhesive force and the like of the low-temperature conductive silver paste are provided.
At present, most of silver pastes used in domestic markets are domestic silver pastes, and a small part of silver pastes are foreign products such as DuPont, Changxing, Eschson and the like, so that the following problems mainly exist: silver paste has poor oxidation resistance, silver wires are easy to discolor, so that the storage time of electronic or printed circuit board products cannot be too long, and the phenomenon of abnormal conductivity of conductive circuits is easy to occur; the oxidation resistance of individual silver paste is good, but the acid and alkali resistance is poor, so that the silver wires partially fall off, and the stability of electronic products is influenced.
Therefore, the development of the low-temperature conductive silver paste with good oxidation resistance and acid and alkali resistance is of great significance.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the anti-oxidation low-temperature conductive silver paste with small paste impedance, excellent anti-oxidation performance and good adhesive force and the preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the anti-oxidation low-temperature conductive silver paste comprises the following raw materials in percentage by mass: 6-8% of high molecular resin; 50-60% of metal silver powder; 0.5 to 1.0 percent of curing agent; 0.5 to 1.0 percent of antioxidant auxiliary agent; 2 to 10 percent of thickening agent; 30-40% of solvent.
The silver powder is at least one of flake silver powder or sphere-like silver powder.
The flake silver powder has the D50 of 1.80-5.0 mu m and the tap density of 1.70-2.50g/cm3(ii) a The D50 of the quasi-spherical silver powder is 0.8-2.5 μm, and the tap density is 3.0-4.50 g-cm3。
The high polymer resin is at least one of polyurethane resin, polyester resin, acrylic resin, epoxy resin or vinyl chloride-vinyl acetate resin.
The curing agent is a closed isocyanate curing agent, the isocyanate NCO content is 6.5-12%, and the deblocking temperature is 90-120 ℃.
The antioxidant auxiliary agent is at least one of benzotriazole derivatives, benzotriazole BTA, tolyltriazole TTA, phosphate, barium petroleum sulfonate or benzoate.
The thickening agent is at least one of graphite, carbon black, polyamide wax, modified bentonite or hydroxyethyl cellulose.
The organic solvent comprises at least one of dimethyl glutarate, dimethyl succinate, dimethyl adipate, 1-4 butyl lactone, propylene glycol methyl ether acetate or DBE.
A preparation method of antioxidant low-temperature conductive silver paste comprises the following steps:
s1, heating the solvent to 60-95 ℃, then adding the polymer resin, stirring until the polymer resin is completely dissolved, filtering and removing impurities on a 300-400-mesh screen cloth, standing and cooling to room temperature to obtain an organic carrier;
s2, adding the silver powder, the curing agent, the antioxidant auxiliary agent and the thickening agent into the organic carrier obtained in the S1, and uniformly dispersing to obtain a coarse slurry;
and S3, grinding and rolling the crude slurry obtained in the step S2 to obtain silver paste, namely the antioxidant low-temperature conductive silver paste.
And grinding and rolling the rough pulp in the S3 by using a three-roll mill, wherein the obtained antioxidant low-temperature conductive silver paste has the fineness of 3-5 mu m and the viscosity of 20000mPa & S-30000mPa & S.
The beneficial technical effects of the invention are as follows: the oxidation resistance of the low-temperature conductive silver paste is improved, so that the low-temperature conductive silver paste can be used in a complex environment, and the service cycle of a product is longer; mainly because can promote the anti-oxidant ability of metal through adding metal antioxidant, the anti-oxidant molecule takes place physical adsorption through electrostatic attraction and intermolecular force with the metal surface, some organic functional groups and metal ion carry out the chelation, form the chemical bond, consequently, the anti-oxidant passes through physics or chemical adsorption, form the very thin film of one deck at the metal surface, form fine and close and firm film, protection silver thick liquid avoids silver powder particle surface to suffer external impurity, grease, the erosion of factors such as steam, thereby reach and promote the anti-oxidant ability of silver thick liquid, promote the cycle of silver thick liquid product, the application field of silver thick liquid has been widened.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1:
a preparation method of the antioxidant low-temperature conductive silver paste comprises the following steps:
according to the mass percentage, 50 percent of silver powder, 8 percent of polymer resin, 0.5 percent of curing agent, 0.5 percent of antioxidant auxiliary agent, 10 percent of thickening agent and 31 percent of solvent are weighed. The silver powder is flake silver powder, the particle diameter of the silver powder is 4.5 mu m, and the tap density is 2.48g/cm3(ii) a The high polymer resin is polyurethane resin TPU 550; the curing agent is an Asahi formed MF-K60X, and is deblocked at 90 ℃; the antioxidant auxiliary agent is a benzotriazole derivative; the thickening agent is carbon black; the solvent is DBE.
Preparing a carrier: weighing 8% of polyurethane TPU550 and 31% of DBE, introducing the polyurethane TPU550 and the 31% of DBE into a heating kettle, heating the heating kettle to 85 ℃, keeping the temperature constant, and filtering and removing impurities on a 300-mesh 400-mesh screen cloth after the polyurethane resin is completely dissolved to obtain a carrier;
preparing silver paste: weighing the flaky metal silver powder, the obtained organic carrier, the curing agent, the thickening agent and the benzene antioxidant auxiliary agent, and placing the mixture into a centrifugal dispersion machine for high-speed dispersion to obtain uniform slurry;
production of silver paste: grinding the slurry in a three-roll mill for 6 times, and finely adjusting by using a roller to control the fineness of the silver paste to be below 5 mu m and the viscosity to be 22300mPa & s, thereby finally obtaining the antioxidant low-temperature halogen-free conductive silver paste.
Example 2:
a preparation method of the antioxidant low-temperature conductive silver paste comprises the following steps:
according to the natureWeighing 55% of metal silver powder, 6% of polymer resin, 1.0% of curing agent, 1.0% of antioxidant additive, 5% of thickening agent and 32% of solvent. The silver powder is flake silver powder, the particle diameter of the silver powder is 3.83 mu m, and the tap density is 2.03g/cm3(ii) a The high polymer resin is-polyester resin 270; the curing agent is a blocked isocyanate curing agent which is prepared by Asahi chemical MF-B60X and is deblocked at 120 ℃; the antioxidant auxiliary agent is methylbenzotriazole; the thickening agent is carbon black; the solvent is a mixed solvent of dimethyl succinate and dimethyl adipate with the ratio of 1: 1.
Preparing a carrier: weighing 6% of polyester 270 and 32% of mixed solvents, namely dimethyl succinate and dimethyl adipate, introducing into a heating kettle, heating to 85 ℃, keeping the temperature constant, and filtering and removing impurities on a 300-mesh 400-mesh screen cloth after resin is completely dissolved to obtain a carrier;
preparing silver paste: weighing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent, and placing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent in a centrifugal dispersion machine for high-speed dispersion to obtain uniform slurry;
production of silver paste: grinding the slurry in a three-roll mill for 6 times, and finely adjusting by using a roller to control the fineness of the silver paste to be less than 5 mu m and the viscosity to be 21170mPa & s, namely the antioxidant low-temperature halogen-free silver paste.
Example 3:
a preparation method of the antioxidant low-temperature conductive silver paste comprises the following steps:
according to the mass percentage, 60 percent of silver powder, 6 percent of polymer resin, 1.0 percent of curing agent, 1.0 percent of antioxidant auxiliary agent, 2 percent of thickening agent and 30 percent of solvent are weighed. The metal silver powder is spherical-like silver powder, the particle diameter of the metal silver powder is 2.01 mu m, and the tap density is 3.98g/cm3(ii) a The high molecular resin is hydroxyl modified ternary vinyl chloride-vinyl acetate copolymer (VAGH); the curing agent is an Asahi formed MF-K60X which is deblocked at 90 ℃; the antioxidant auxiliary agent is benzotriazole; the thickening agent is carbon black; the solvent is a mixed solvent of 1-4 butyl lactone and propylene glycol methyl ether acetate, and the proportion of the mixed solvent is 2: 1.
preparing a carrier: weighing 6% of hydroxyl modified ternary vinyl chloride-vinyl acetate copolymer (VAGH), 30% of mixed solvent 1-4 butyrolactone and propylene glycol methyl ether acetate, introducing into a heating kettle, heating to 85 ℃, keeping the temperature, and filtering and removing impurities on a 300-mesh 400-mesh screen cloth after the resin is completely dissolved to obtain a carrier;
preparing silver paste: weighing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent, and placing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent in a centrifugal dispersion machine for high-speed dispersion to obtain uniform slurry;
production of silver paste: grinding the slurry in a three-roll mill for 6 times, and finely adjusting by using a roller to control the fineness of the silver paste to be less than 5 mu m and the viscosity to be 22500mPa & s, namely the antioxidant low-temperature halogen-free conductive silver paste.
Comparative example 1:
according to the mass percentage, 50 percent of silver powder, 8 percent of polymer resin, 0.5 percent of curing agent, 10 percent of thickening agent and 31.5 percent of solvent are weighed. The silver powder is flake silver powder, the particle diameter of the silver powder is 4.5 mu m, and the tap density is 2.48g/cm3(ii) a The high polymer resin is polyurethane resin TPU 550; the curing agent is an Asahi formed MF-K60X, and is deblocked at 90 ℃; the thickening agent is carbon black; the solvent is DBE.
Preparing a carrier: weighing 8% of polyurethane TPU550 and 31.5% of DBE, introducing the polyurethane TPU550 and the 31.5% of DBE into a heating kettle, heating the heating kettle to 85 ℃, keeping the temperature constant, and filtering and removing impurities on a 300-mesh 400-mesh screen cloth after the polyurethane resin is completely dissolved to obtain a carrier;
preparing silver paste: weighing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent, and placing the flaky metal silver powder, the organic carrier, the curing agent, the thickening agent and the antioxidant auxiliary agent in a centrifugal dispersion machine for high-speed dispersion to obtain uniform slurry;
production of silver paste: grinding the slurry in a three-roll mill for 6 times, and finely adjusting by using a roller to control the fineness of the silver paste to be less than 5 microns and 23000mPa & s, namely the anti-oxidation low-temperature conductive silver paste.
The difference between the examples 1, 2 and 3 and the comparative example 1 lies in that the examples 1, 2 and 3 are respectively different from the comparative example 1 in that different antioxidant additives are added, the organic matters are partially the same, and the metal silver powders are all flake-shaped metal silver powders under the same system.
And (3) printing the paste prepared in the examples 1-3 and the paste prepared in the comparative example 1 on a PET (polyethylene terephthalate) base material by adopting screen printing, wherein the printed lines have the line width of 0.3mm and the line length of 500mm, and drying at 150 ℃ for 30-60 min. Then, the oxidation resistance test was performed, and the test results are shown in table 1.
The anti-oxidation test method comprises the following steps: by adopting acid-base artificial sweat, an external impurity pollution source in the environment is simulated, the surface of a silver paste printing coating is polluted, then the silver paste printing coating is placed in an environment with certain temperature and humidity (the temperature is 70 ℃/the humidity is 90% RH), the change condition of silver line impedance in different time is tested, the electrical property influence of the acid sweat and the alkaline sweat on low-temperature silver paste is investigated, and the oxidation resistance of the silver paste is evaluated.
TABLE 1 Performance test results of examples 1 to 3 and comparative example 1 are shown in the table (Ω)
From the test results, it can be seen that in the examples 1, 2 and 3 of the antioxidant low-temperature conductive silver paste prepared by the method, compared with the comparative example 1, the antioxidant performance of the conductive silver paste is very excellent, and the resistance of the silver paste is hardly increased under different storage times. Example 1 has been developed into a low temperature conductive silver paste product for mass production by customers, mainly for keyboard and membrane switch applications.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The anti-oxidation low-temperature conductive silver paste is characterized by comprising the following raw materials in percentage by mass: 6-8% of high molecular resin; 50-60% of metal silver powder; 0.5 to 1.0 percent of curing agent; 0.5 to 1.0 percent of antioxidant auxiliary agent; 2 to 10 percent of thickening agent; 30-40% of solvent.
2. The conductive silver paste of claim 1, wherein said silver powder is at least one of flake silver powder or sphere-like silver powder.
3. The conductive silver paste of claim 2, wherein the flake silver powder has a D50 of 1.80 to 5.0 μm and a tap density of 1.70 to 2.50g/cm3(ii) a The D50 of the sphere-like silver powder is 0.8-2.5 mu m, and the tap density is 3.0-4.50g/cm3。
4. The conductive silver paste of claim 1, wherein the polymeric resin is at least one of a polyurethane resin, a polyester resin, an acrylic resin, an epoxy resin, or a vinyl chloride-vinyl acetate resin.
5. The conductive silver paste of claim 1, wherein the curing agent is a blocked isocyanate curing agent having an NCO content of 6.5-12% and a deblocking temperature of 90-120 ℃.
6. The conductive silver paste of claim 1, wherein the antioxidant additive is at least one of benzotriazole derivatives, benzotriazole BTA, benzotriazole TTA, phosphate, barium petroleum sulfonate, or benzoate.
7. The conductive silver paste of claim 1, wherein the thickener is at least one of graphite, carbon black, polyamide wax, modified bentonite, or hydroxyethyl cellulose.
8. The conductive silver paste of claim 1, wherein the organic solvent comprises at least one of dimethyl glutarate, dimethyl succinate, dimethyl adipate, 1-4 butyl lactone, propylene glycol methyl ether acetate, or DBE.
9. The preparation method of the antioxidant low-temperature conductive silver paste as set forth in any one of claims 1 to 8, wherein the preparation method comprises the following steps:
s1, heating the solvent to 60-95 ℃, then adding the polymer resin, stirring until the polymer resin is completely dissolved, filtering and removing impurities on a 300-400-mesh screen cloth, standing and cooling to room temperature to obtain an organic carrier;
s2, adding the silver powder, the curing agent, the antioxidant auxiliary agent and the thickening agent into the organic carrier obtained in the S1, and uniformly dispersing to obtain a coarse slurry;
and S3, grinding and rolling the crude slurry obtained in the step S2 to obtain silver paste, namely the antioxidant low-temperature conductive silver paste.
10. The antioxidant low-temperature conductive silver paste as claimed in claim 9, wherein: and grinding and rolling the rough pulp in the S3 by using a three-roll mill, wherein the obtained antioxidant low-temperature conductive silver paste has the fineness of 3-5 mu m and the viscosity of 20000mPa & S-30000mPa & S.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113517093A (en) * | 2021-04-22 | 2021-10-19 | 苏州海力金属粉体材料有限公司 | Preparation method of spherical silver powder conductive paste |
CN114141404A (en) * | 2021-11-22 | 2022-03-04 | 苏州市贝特利高分子材料股份有限公司 | High-conductivity high-flexibility low-temperature silver paste |
CN114709005A (en) * | 2022-03-29 | 2022-07-05 | 深圳市百柔新材料技术有限公司 | Silver paste for flexible transparent conductive film metal grid, preparation method and application thereof |
WO2023045348A1 (en) * | 2021-09-26 | 2023-03-30 | 西安隆基乐叶光伏科技有限公司 | Antioxidant conductive copper paste, preparation method therefor, and use thereof |
CN116092721A (en) * | 2022-12-23 | 2023-05-09 | 苏州英纳电子材料有限公司 | High-adhesion low-resistance silver paste and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113517093A (en) * | 2021-04-22 | 2021-10-19 | 苏州海力金属粉体材料有限公司 | Preparation method of spherical silver powder conductive paste |
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CN116092721A (en) * | 2022-12-23 | 2023-05-09 | 苏州英纳电子材料有限公司 | High-adhesion low-resistance silver paste and preparation method thereof |
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Application publication date: 20210126 |