CN115910426A - High-thixotropy conductive silver paste and preparation method thereof - Google Patents

High-thixotropy conductive silver paste and preparation method thereof Download PDF

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CN115910426A
CN115910426A CN202310020091.4A CN202310020091A CN115910426A CN 115910426 A CN115910426 A CN 115910426A CN 202310020091 A CN202310020091 A CN 202310020091A CN 115910426 A CN115910426 A CN 115910426A
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parts
silver paste
conductive
calcium carbonate
preparation
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殷文钢
冯大伟
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Nano Top Electronic Technology Co ltd
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Nano Top Electronic Technology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/50Photovoltaic [PV] energy

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Abstract

The invention provides a high-thixotropy conductive silver paste and a preparation method thereof, wherein the conductive silver paste consists of 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic auxiliary agent, 1-2 parts of calcium carbonate and 1-2 parts of additive, and the preparation method comprises four steps of material preparation, adhesive preparation, conductive silver paste preparation and conductive silver paste preparation.

Description

High-thixotropy conductive silver paste and preparation method thereof
Technical Field
The invention relates to the technical field of conductive silver paste, in particular to high-thixotropy conductive silver paste and a preparation method thereof.
Background
In recent years, conductive silver paste is widely used in printed electronics industry, such as integrated circuits, solar cells, radio frequency identification tags, thin film transistors, biosensors, and the like. The conductive silver paste is an electronic paste which is printed on insulators such as PET (polyethylene terephthalate), ceramics, glass, paperboards and the like to enable the insulators to have the current transmission and static charge removal capabilities, and is a key raw material of electronic products such as various electronic components, electrodes and the like;
the thixotropy of the conductive silver paste has great influence on the yield of circuit printing, for example, viscosity, cohesiveness, adhesive force, leveling property, film forming property, volatility of a solvent and the like all influence the printing performance of the circuit, so that the conductive circuit falls off from a printing stock, the conductive circuit is scrapped, and the thixotropy of the conductive silver paste needs to be improved;
however, in the prior art, the thixotropy of the conductive silver paste is improved by adding a thixotropic auxiliary agent in the preparation process of the conductive silver paste, but the thixotropic auxiliary agent has some limitations, and the performance of the conductive silver paste is affected with the increase of the amount of the thixotropic auxiliary agent, so that the conductive silver paste with high thixotropy and the preparation method thereof are provided to solve the problems in the prior art.
Disclosure of Invention
In order to solve the problems, the invention aims to provide the high-thixotropy conductive silver paste and the preparation method thereof.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: the high-thixotropy conductive silver paste and the preparation method thereof comprise the following raw materials in parts by weight: 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic additive, 1-2 parts of calcium carbonate and 1-2 parts of additive.
The further improvement is that: the calcium carbonate is 800-mesh calcium carbonate powder.
The further improvement lies in that: the epoxy resin is bisphenol A type epoxy resin.
The further improvement is that: the thixotropic auxiliary agent is gas-phase SiO 2
The further improvement is that: the additive is polyethylene glycol.
The preparation method of the high-thixotropy conductive silver paste comprises the following steps:
step one, material preparation
Preparing materials according to parts by weight: 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic aid, 1-2 parts of calcium carbonate and 1-2 parts of additive, and then pretreating part of the materials;
step two, preparing the adhesive
Accurately weighing the epoxy resin, the solvent, the calcium carbonate and the conductive promoter according to the weight parts in the step one, firstly placing the epoxy resin into a reaction container, then adding the solvent, the calcium carbonate and the conductive promoter, then heating to 80 ℃, keeping the temperature unchanged, stirring and mixing the epoxy resin, the calcium carbonate and the conductive promoter through the reaction container, fully mixing the epoxy resin, the solvent, the calcium carbonate and the conductive promoter to obtain a mixture, and then carrying out secondary treatment on the mixture to obtain the adhesive;
step three, silver paste preparation
Accurately weighing the silver powder, the curing agent and the thixotropic auxiliary agent according to the weight parts in the first step, putting the silver powder, the curing agent and the thixotropic auxiliary agent and the adhesive in the second step into a mixer, mixing the silver powder, the curing agent and the thixotropic auxiliary agent by the mixer, adding the additive after fully mixing, mixing again, and dispersing the mixture at a high speed by using a high-speed dispersion machine after uniformly mixing to obtain uniform slurry;
step four, conductive silver paste preparation
And (3) grinding the slurry obtained in the third step by using a three-roll grinder, adding a solvent for fine adjustment in the grinding process to enable the fineness of the silver paste to reach below 10 mu m, stopping grinding, and taking out the material to finish the preparation of the high-thixotropy conductive silver paste.
The further improvement lies in that: in the first step, calcium carbonate is pretreated, specifically, the calcium carbonate is ground by a grinding machine, and is sieved by a 800-mesh screen after grinding to obtain 800-mesh calcium carbonate.
The further improvement is that: in the second step, the secondary treatment specifically comprises: and filtering and removing impurities from the mixture by using 500-mesh filter screen cloth.
The invention has the beneficial effects that: this kind of electrically conductive silver thick liquid of high thixotropy and preparation method adopt 800 mesh calcium carbonate as packing, and adopt the resin system of low viscosity, promote the thixotropy of electrically conductive silver thick liquid self from this, and can reduce the addition of thixotropic auxiliary agent, when guaranteeing electrically conductive silver thick liquid high thixotropy from this, can also avoid reducing the problem of electrically conductive silver thick liquid conductivity because of the too big problem that leads to of thixotropic auxiliary agent addition, reduce its self problem because of promoting electrically conductive silver thick liquid thixotropy among the solution prior art, the rethread adds a small amount of electrically conductive promoter, can not influence the performance of electrically conductive silver thick liquid self, promote the electric conductive property of electrically conductive silver thick liquid simultaneously.
Drawings
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example one
According to the illustration in fig. 1, the embodiment provides a high thixotropy conductive silver paste and a preparation method thereof, wherein the conductive silver paste comprises the following raw materials in parts by weight: 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic auxiliary agent, 1-2 parts of calcium carbonate and 1-2 parts of additive, wherein the calcium carbonate is 800-mesh calcium carbonate powder, the epoxy resin is bisphenol A type epoxy resin, and the thixotropic auxiliary agent is gas-phase SiO 2 The additive is polyethylene glycol, the solvent is ethylene glycol monobutyl ether acetate, the conductive promoter is NY-801 conductive promoter, and the curing agent is closed melamine curing agent.
The preparation method of the high-thixotropy conductive silver paste comprises the following steps:
step one, material preparation
Preparing materials according to parts by weight: 25-35 parts of epoxy resin, 55-65 parts of silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic aid, 1-2 parts of calcium carbonate and 1-2 parts of additive, and then pretreating part of materials, wherein in the first step, the calcium carbonate is pretreated, and specifically, the calcium carbonate is ground by a grinding machine and sieved by a 800-mesh screen after grinding to obtain 800-mesh calcium carbonate;
step two, preparing the adhesive
Accurately weighing the epoxy resin, the solvent, the calcium carbonate and the conductive accelerator according to the parts by weight in the first step, firstly placing the epoxy resin into a reaction container, then adding the solvent, the calcium carbonate and the conductive accelerator, then heating to 80 ℃, keeping the temperature unchanged, stirring and mixing the epoxy resin, the solvent, the calcium carbonate and the conductive accelerator through the reaction container, fully mixing the epoxy resin, the calcium carbonate and the conductive accelerator to obtain a mixture, and then carrying out secondary treatment on the mixture to obtain the adhesive, wherein in the second step, the secondary treatment specifically comprises the following steps: filtering the mixture by using 500-mesh filter screen cloth to remove impurities;
step three, silver paste preparation
Accurately weighing the silver powder, the curing agent and the thixotropic auxiliary agent according to the weight parts in the first step, putting the silver powder, the curing agent and the thixotropic auxiliary agent and the adhesive in the second step into a mixer, mixing the silver powder, the curing agent and the thixotropic auxiliary agent by the mixer, adding the additive after fully mixing, mixing again, and dispersing the mixture at a high speed by using a high-speed dispersion machine after uniformly mixing to obtain uniform slurry;
step four, conductive silver paste preparation
And (3) grinding the slurry obtained in the third step by using a three-roll grinder, adding a solvent for fine adjustment in the grinding process to enable the fineness of the silver paste to reach below 10 mu m, stopping grinding, and taking out the material to finish the preparation of the high-thixotropy conductive silver paste.
Example two
The embodiment provides a high-thixotropy conductive silver paste and a preparation method thereof, wherein the high-thixotropy conductive silver paste comprises the following raw materials in parts by weight: 25 parts of epoxy resin, 65 parts of metal silver powder, 3 parts of solvent, 1 part of curing agent, 1 part of conductive accelerator, 1 part of thixotropic auxiliary agent, 2 parts of calcium carbonate and 1 part of additive, wherein the calcium carbonate is 800-mesh calcium carbonate powder, the epoxy resin is bisphenol A type epoxy resin, and the thixotropic auxiliary agent is gasPhase SiO 2 The additive is polyethylene glycol, the solvent is ethylene glycol butyl ether acetate, the conductive promoter is NY-801 conductive promoter, and the curing agent is a closed melamine curing agent.
The preparation method of the high-thixotropy conductive silver paste is the same as the first embodiment.
EXAMPLE III
The embodiment provides a high-thixotropy conductive silver paste and a preparation method thereof, wherein the high-thixotropy conductive silver paste comprises the following raw materials in parts by weight: 35 parts of epoxy resin, 55 parts of metal silver powder, 5 parts of solvent, 1 part of curing agent, 0.5 part of conductive accelerator, 0.5 part of thixotropic auxiliary agent, 2 parts of calcium carbonate and 1 part of additive, wherein the calcium carbonate is 800-mesh calcium carbonate powder, the epoxy resin is bisphenol A type epoxy resin, and the thixotropic auxiliary agent is gas-phase SiO 2 The additive is polyethylene glycol, the solvent is ethylene glycol butyl ether acetate, the conductive promoter is NY-801 conductive promoter, and the curing agent is a closed melamine curing agent.
The preparation method of the high-thixotropy conductive silver paste is the same as that of the first embodiment.
Example four
According to fig. 1, this embodiment proposes a method for preparing a conductive silver paste with high thixotropy, which includes the following steps:
step one, material preparation
Preparing materials according to parts by weight: 35 parts of epoxy resin, 55 parts of metal silver powder, 5 parts of solvent, 1 part of curing agent, 0.5 part of conductive accelerator, 0.5 part of thixotropic aid, 2 parts of calcium carbonate and 1 part of additive, and then pretreating part of the materials, wherein in the embodiment, only the calcium carbonate needs to be pretreated, specifically, the calcium carbonate is ground by a grinding machine and sieved by a 800-mesh sieve to obtain 800-mesh calcium carbonate, part of calcium carbonate which does not pass through can be generated in the sieving process, the calcium carbonate is ground again by the grinding machine, and the ground calcium carbonate is sieved by the 800-mesh sieve;
step two, preparing the adhesive
Accurately weighing the epoxy resin, the solvent, the calcium carbonate and the conductive accelerator according to the parts by weight in the first step, firstly placing the epoxy resin into a reaction container, wherein the reaction container has the functions of stirring and heating, and then adding the solvent, the calcium carbonate and the conductive accelerator, wherein the solvent is ethylene glycol butyl ether acetate, and the solvent can also be used as a diluent, further adding the calcium carbonate as a filler in the preparation process of the adhesive, and pretreating the calcium carbonate to improve the mesh number of the filler, so that the thixotropy of a mixed glue solution is improved along with the increase of the mesh number of the filler, namely in the embodiment, the thixotropy of the adhesive is adjusted by adopting a fine filler, so that the thixotropy of the conductive silver paste prepared subsequently is improved, and then adding a small amount of the conductive accelerator does not influence the performance of the conductive silver paste, and simultaneously improves the conductivity of the conductive silver paste;
specifically, the temperature in the reaction container is raised to 80 ℃, the temperature is kept unchanged, the epoxy resin is stirred and mixed through the reaction container, in the mixing process, the epoxy resin is dissolved and diluted by a solvent, namely, the epoxy resin is diluted to 1000/mPa · s viscosity, in the embodiment, a resin system with low viscosity is adopted, the thixotropy of the materials can be improved, namely, after the epoxy resin is fully mixed, a mixture is obtained, and then the mixture is subjected to secondary treatment to obtain the adhesive, wherein in the second step, the secondary treatment specifically comprises the following steps: filtering and removing impurities from the mixture by using 500-mesh filter screen cloth;
step three, silver paste preparation
Accurately weighing the silver powder, the curing agent and the thixotropic auxiliary agent according to the weight ratio in the first step, placing the silver powder, the curing agent and the thixotropic auxiliary agent and the adhesive in the second step into a mixer, mixing the silver powder, the curing agent and the thixotropic auxiliary agent by the mixer, adding an additive after fully mixing the silver powder, the curing agent and the thixotropic auxiliary agent, and mixing the mixture again, wherein the additive is polyethylene glycol which has good lubricity, moisture retention property, dispersibility and adhesiveness and is used as a softening agent in the embodiment to improve the comprehensive performance of the silver paste;
step four, conductive silver paste preparation
And (3) grinding the slurry obtained in the third step by using a three-roll grinder, adding a solvent for fine adjustment in the grinding process to enable the fineness of the silver paste to reach below 10 mu m, and taking out the material to finish the preparation of the high-thixotropy conductive silver paste.
Specifically, in the embodiment, the conductive silver paste itself is composed of a conductive filler (metal silver powder), an adhesive, a solvent and an additive, and the metal silver powder is a flake silver powder, which has high thixotropy and is more favorable for forming a space network structure.
According to the invention, 800-mesh calcium carbonate is added as a filler to improve the thixotropy of the prepared adhesive, and a low-viscosity resin system is adopted to improve the thixotropy of the material so as to reduce the addition of the thixotropic additive 2 Then in the preparation process of the conductive silver paste, gas-phase SiO is generated along with the thixotropic additive 2 Increase in the amount of use, i.e. gas phase SiO 2 The mass fraction of the conductive silver paste is improved, the thixotropy of the conductive silver paste is increased, the use amount is increased, the viscosity of the system is obviously increased, the conductivity of the conductive silver paste is reduced, the gloss of the paste is influenced, namely, the high thixotropy is achieved, and the performance of the conductive silver paste is reduced.
The foregoing shows and describes the general principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. The high-thixotropy conductive silver paste is characterized in that: the composite material consists of the following raw materials in parts by weight: 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic additive, 1-2 parts of calcium carbonate and 1-2 parts of additive.
2. The high thixotropy conductive silver paste of claim 1, wherein: the calcium carbonate is 800-mesh calcium carbonate powder.
3. The high thixotropy conductive silver paste of claim 1, wherein: the epoxy resin is bisphenol A type epoxy resin.
4. The high thixotropic conductive silver paste of claim 1, wherein: the thixotropic auxiliary agent is gas-phase SiO 2
5. The high thixotropy conductive silver paste of claim 1, wherein: the additive is polyethylene glycol.
6. The preparation method of the high-thixotropy conductive silver paste applied to the material of claim 1 is characterized in that: the method comprises the following steps:
step one, material preparation
Preparing materials according to parts by weight: 25-35 parts of epoxy resin, 55-65 parts of metal silver powder, 3-5 parts of solvent, 1-2 parts of curing agent, 0.5-1 part of conductive accelerator, 0.5-1 part of thixotropic auxiliary agent, 1-2 parts of calcium carbonate and 1-2 parts of additive, and then pretreating part of the materials;
step two, preparing the adhesive
Accurately weighing the epoxy resin, the solvent, the calcium carbonate and the conductive promoter according to the weight parts in the step one, firstly placing the epoxy resin into a reaction container, then adding the solvent, the calcium carbonate and the conductive promoter, then heating to 80 ℃, keeping the temperature unchanged, stirring and mixing the epoxy resin, the calcium carbonate and the conductive promoter through the reaction container, fully mixing the epoxy resin, the solvent, the calcium carbonate and the conductive promoter to obtain a mixture, and then carrying out secondary treatment on the mixture to obtain the adhesive;
step three, silver paste preparation
Accurately weighing the silver powder, the curing agent and the thixotropic auxiliary agent according to the weight parts in the first step, putting the silver powder, the curing agent and the thixotropic auxiliary agent and the adhesive in the second step into a mixer, mixing the silver powder, the curing agent and the thixotropic auxiliary agent by the mixer, adding the additive after fully mixing, mixing again, and dispersing the mixture at a high speed by using a high-speed dispersion machine after uniformly mixing to obtain uniform slurry;
step four, conductive silver paste preparation
And (4) grinding the slurry obtained in the third step by a three-roll grinder, adding a solvent for fine adjustment in the grinding process to enable the fineness of the silver paste to reach below 10 mu m, stopping grinding, taking out the material, and completing the preparation of the high-thixotropy conductive silver paste.
7. The preparation method of the high thixotropy conductive silver paste according to claim 6, characterized in that: in the first step, calcium carbonate is pretreated, specifically, the calcium carbonate is ground by a grinding machine, and is sieved by a 800-mesh screen after grinding to obtain 800-mesh calcium carbonate.
8. The preparation method of the high thixotropy conductive silver paste according to claim 6, characterized in that: in the second step, the secondary treatment specifically comprises: and filtering and removing impurities from the mixture by using 500-mesh filter screen cloth.
CN202310020091.4A 2023-01-06 2023-01-06 High-thixotropy conductive silver paste and preparation method thereof Pending CN115910426A (en)

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