CN116130143A - High-temperature-resistant elastic conductive silver paste and preparation method thereof - Google Patents
High-temperature-resistant elastic conductive silver paste and preparation method thereof Download PDFInfo
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- CN116130143A CN116130143A CN202211742124.8A CN202211742124A CN116130143A CN 116130143 A CN116130143 A CN 116130143A CN 202211742124 A CN202211742124 A CN 202211742124A CN 116130143 A CN116130143 A CN 116130143A
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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
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention discloses high-temperature-resistant elastic conductive silver paste and a preparation method thereof, and belongs to the technical field of conductive silver paste. The adhesive consists of the following raw materials in parts by weight: 5-15 parts of modified epoxy resin, 0.5-9 parts of curing agent, 1-5 parts of epoxy resin, 5-10 parts of diluent, 0.1-0.5 part of silane coupling agent, 0.01-0.2 part of curing accelerator, 0.01-0.5 part of dispersing agent, 0.2-2 parts of thixotropic agent and 70-90 parts of conductive filler. The change rate of the mechanical property and the electrical property at 300 ℃/30 minutes is less than 5%; the elastic performance is good, and the Shore hardness is 80-90; excellent in conductivity and volume resistivity of 1X 10 ‑5 ‑5×10 ‑6 Omega cm. The method can be completed by using general industrial equipment, has low requirements on the complexity of the equipment, is easy to operate, has stable process and high production efficiency, and is suitable for batch industrial production.
Description
Technical Field
The invention relates to the technical field of conductive silver paste, in particular to high-temperature-resistant elastic conductive silver paste and a preparation method thereof.
Background
At present, the conductive silver paste for electronic products has the advantages of high connection reliability, low processing temperature, environmental friendliness and the like, and gradually replaces the traditional lead-containing solder. The conductive silver paste is uniformly mixed and solidified with the conductive particles through the matrix resin to form a conductive path to realize conductive performance, and the bonding material has certain mechanical performance and thermal performance. The conductive silver paste is widely applied to packaging and bonding of liquid crystal display screens, LEDs, IC chips, printed circuit boards, radio frequency identification electronic elements and components, and relates in part to high-temperature use environments. Most of the existing conductive silver paste has poor electrical property and mechanical property after high-temperature environment or poor high-temperature resistance and high brittleness after solidification, so that the conductive silver paste cannot exert the effect of gluing electronic component materials under high-temperature environment and cannot meet the shock resistance and vibration requirements of electronic products, and therefore, the research on the use of the conductive silver paste capable of resisting high temperature and elastic at a certain temperature is necessary.
The research of the traditional conductive silver paste is mainly focused on improving the conductive performance or the adhesive performance, and has few excellent electrical properties while meeting the use environment requirements of electronic devices by resisting high temperature and welding heat. The invention application CN115312229A, a geothermal film conductive silver paste and a preparation method thereof, can only provide a conductive silver paste resistant to 50 ℃. Other disclosed high-temperature resistant conductive silver paste adopts silver nanowires and nano silver powder, and has complex process and higher cost; some of the silver and other metal mixed technologies are adopted, the high temperature resistance is not high, the temperature cannot exceed 180 ℃, and the conductivity is not ideal.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of high-temperature-resistant elastic conductive silver paste, which is realized by the following technical scheme:
the high-temperature-resistant elastic conductive silver paste comprises the following raw materials in parts by weight: 5-15 parts of modified epoxy resin, 0.5-9 parts of curing agent, 1-5 parts of epoxy resin mixture, 5-10 parts of diluent, 0.1-0.5 part of silane coupling agent, 0.01-0.2 part of curing accelerator, 0.01-0.5 part of dispersing agent, 0.2-2 parts of thixotropic agent and 70-90 parts of conductive filler.
The modified epoxy resin is organic silicon epoxy resin or organic boron epoxy resin, the viscosity is 1000-6000 mPa.s, and the epoxy value is 0.30-0.87; the epoxy resin is alicyclic glycidyl ester type epoxy resin; the curing agent is at least one of DDS, MNA, PDMA; the diluent is at least one of p-tert-butylphenyl glycidyl ether, phenyl glycidyl ether and butanediol glycidyl ether; the coupling agent is a silane coupling agent. The curing accelerator is at least one of diethyl tetramethyl imidazole, DMP-30 and 2E4 MI.
The invention also discloses a preparation method of the high-temperature-resistant elastic conductive silver paste, which comprises the following steps:
(1) 5-15 parts of modified epoxy resin and 1-5 parts of epoxy resin are heated at 55-80 ℃ for 30-180 minutes. Adding 5-10 parts of diluent, and centrifuging and dispersing parameters: (80-1400) revolutions per minute, (30-120) seconds; (2) adding 0.5-9 parts of curing agent, 0.01-0.2 part of curing accelerator, 0.1-0.5 part of silane coupling agent, 0.01-0.5 part of dispersing agent and 0.2-2 parts of thixotropic agent, stirring, and carrying out three-roller grinding, wherein the roller spacing is 5-30 micrometers, and grinding is carried out for 2-3 times to obtain a resin matrix;
(3) adding 70-90 parts of silver powder into the resin matrix, and centrifugally dispersing (80-1400) for (30-120) seconds to obtain the high-temperature-resistant elastic conductive silver paste.
Compared with the prior art, the invention has the following advantages:
(1) The high-temperature resistant elastic conductive silver paste has excellent high-temperature resistance, and the mechanical property and the electrical property change rate of 300 ℃/30 minutes are less than 5%; the elastic performance is good, and the Shore hardness is 80-90; excellent in conductivity and volume resistivity of 1X 10 -5 -5×10 -6 Ω·cm。
(2) The high-temperature-resistant elastic conductive silver paste can meet the requirements of electronic products on high conductivity, high heat resistance, heat conduction, impact resistance and the like of the conductive silver paste. The conductive silver paste has good technological performance, easy construction, high production efficiency and higher technical economy.
(3) The preparation method of the high-temperature-resistant elastic conductive silver paste can be completed by using general industrial equipment, has low requirements on the complexity of the equipment, is easy to operate, has stable process and high production efficiency, and is suitable for batch industrial production.
Detailed Description
The invention is further described below in connection with specific embodiments.
The high-temperature-resistant elastic conductive silver paste comprises the following raw materials in parts by weight: 5-15 parts of modified epoxy resin, 0.5-9 parts of curing agent, 1-5 parts of epoxy resin, 5-10 parts of diluent, 0.1-0.5 part of silane coupling agent, 0.01-0.2 part of curing accelerator, 0.01-0.5 part of dispersing agent, 0.2-2 parts of thixotropic agent and 70-90 parts of conductive filler.
The modified epoxy resin is one or a mixture of organic silicon epoxy resin and organic boron epoxy resin, the viscosity is 1000-6000 mPa.s, and the epoxy value is 0.30-0.87; the epoxy resin is alicyclic glycidyl ester type epoxy resin; the curing agent is at least one of DDS, MNA, PDMA; the diluent is at least one of p-tert-butylphenyl glycidyl ether, phenyl glycidyl ether and butanediol glycidyl ether; the coupling agent is a silane coupling agent. The curing accelerator is at least one of diethyl tetramethyl imidazole, DMP-30 and 2E4 MI. The dispersant is BYK203. The thixotropic agent is fumed silica. The conductive filler is a mixture of flake silver powder with the purity of more than 99% and nano silver powder, wherein the flake silver powder is at least one of flake silver powder with the average particle size of 1-10 mu m; the nanometer silver powder is at least one silver powder with the average particle size of 50-100 nm.
The preparation method of the high-temperature-resistant elastic conductive silver paste comprises the following steps:
(1) 150g of organosilicon modified epoxy resin and 10g of epoxy resin are heated at 55-80 ℃ for 30-180 minutes. Adding 100g of diluent, centrifugally dispersing (80-1400) r/min (30-120) s;
(2) adding 80g of curing agent, 1g of curing accelerator, 1g of silane coupling agent, 0.1g of dispersing agent and 2g of thixotropic agent, stirring, grinding by three rollers, wherein the roller spacing is 5-30 micrometers, and grinding for 2-3 times to obtain a resin matrix; (3) adding 700g of silver powder into the resin matrix, and centrifugally dispersing (80-1400) for (30-120) seconds to obtain the high-temperature-resistant elastic conductive silver paste.
Example 1
A high-temperature resistant elastic conductive silver paste is composed of the following raw materials: 100g of organosilicon epoxy resin, 10g of R122 epoxy resin, 60g of p-tert-butylphenyl glycidyl ether, 35g of MNA, 1g of KH560 silane coupling agent, 1g of diethyl tetramethylimidazole, 0.1g of BYK203 dispersant, 2g of fumed silica, 820g of flake silver powder and 80g of nano silver powder.
After the conductive silver paste is solidified at 180 ℃/10min plus 250 ℃/20min, the shear strength is 5.2mpa, and the shear strength change rate is 1.9% after 300 ℃/30 min; volume resistivity 1.0 x 10 -5 Omega cm; shore hardness 89.
Example 2
A high-temperature resistant elastic conductive silver paste is composed of the following raw materials: 50g of organic boron epoxy resin, 10g of W-95 epoxy resin, 100g of butanediol glycidyl ether, 10g of DDS curing agent, 1g of KH550 silane coupling agent, cured DMP-30 0.1g,BYK203 0.1g, 2g of fumed silica, 850g of flake silver powder and 50g of nano silver powder.
After 180 ℃/10min plus 280 ℃/20min of conductive silver paste is solidified, the shear strength is 5.5mpa, and the shear strength change rate is 1.4% after 300 ℃/30 min; volume resistivity 9.8×10 -6 Omega cm; shore hardness 89.
Example 3
A high-temperature resistant elastic conductive silver paste is composed of the following raw materials: 120g of organic silicon epoxy resin, 30g of organic boron epoxy resin, 10g of 2021P epoxy resin, 100g of phenyl glycidyl ether, 80g of PDMA, 1g,2E4MI 1g,BYK2030.1g of KH602 silane coupling agent, 2g of fumed silica, 650g of flake silver powder and 50g of nano silver powder.
After 180 ℃/10min+230 ℃/30min of conductive silver paste is solidified, the shear strength is 5.1mpa, and the shear strength change rate is 2.9% after 300 ℃/30 min; volume resistivity 9.1 x 10 -6 Omega cm; shore hardness 87.
The above embodiments are to be construed as examples of the present invention, and the scope of the present invention is defined by the appended claims.
Claims (10)
1. The high-temperature-resistant elastic conductive silver paste is characterized in that: the adhesive consists of the following raw materials in parts by weight: 5-15 parts of modified epoxy resin, 0.5-9 parts of curing agent, 1-5 parts of epoxy resin, 5-10 parts of diluent, 0.1-0.5 part of silane coupling agent, 0.01-0.2 part of curing accelerator, 0.01-0.5 part of dispersing agent, 0.2-2 parts of thixotropic agent and 70-90 parts of conductive filler.
2. The high temperature resistant elastic conductive silver paste of claim 1, wherein the modified epoxy resin is one of a silicone modified epoxy resin, an organoboron epoxy resin, or a mixture thereof.
3. The high temperature resistant elastic conductive silver paste of claim 1, wherein the epoxy resin is a cycloaliphatic glycidyl ester type epoxy resin.
4. The high temperature resistant elastic conductive silver paste of claim 1, wherein the curing agent is at least one of DDS, MNA, PDMA.
5. The high temperature resistant elastic conductive silver paste according to claim 1, wherein the diluent is at least one of p-tert-butylphenyl glycidyl ether, phenyl glycidyl ether, and butanediol glycidyl ether.
6. The high temperature resistant elastic conductive silver paste according to claim 1, wherein the curing accelerator is at least one of diethyl tetramethyl imidazole, DMP-30, 2E4 MI.
7. The high temperature resistant elastic conductive silver paste according to claim 1, wherein the dispersant is BYK203.
8. The high temperature resistant elastic conductive silver paste of claim 1, wherein the thixotropic agent is fumed silica.
9. The high-temperature resistant elastic conductive silver paste according to claim 1, wherein the conductive filler is a mixture of flake silver powder with a purity of 99% or more and nano silver powder, wherein the flake silver powder is selected from at least one of flake silver powder with an average particle size of 1-10 μm; the nanometer silver powder is at least one silver powder with the average particle size of 50-100 nm.
10. A preparation method of high-temperature resistant elastic conductive silver paste is characterized in that,
1) Heating the modified epoxy resin and the epoxy resin, adding a diluent, and uniformly dispersing;
2) Adding a curing agent, a curing accelerator, a silane coupling agent, a dispersing agent and a thixotropic agent, stirring, and carrying out three-roller grinding to obtain a resin matrix;
3) Adding silver powder into the resin matrix, and centrifugally dispersing uniformly to obtain the high-temperature-resistant elastic conductive silver paste.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211742124.8A CN116130143A (en) | 2022-12-30 | 2022-12-30 | High-temperature-resistant elastic conductive silver paste and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211742124.8A CN116130143A (en) | 2022-12-30 | 2022-12-30 | High-temperature-resistant elastic conductive silver paste and preparation method thereof |
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| CN116130143A true CN116130143A (en) | 2023-05-16 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302413A (en) * | 2008-07-01 | 2008-11-12 | 上海上大瑞沪微系统集成技术有限公司 | High temperature resistant epoxide resin conductive adhesive |
| CN103980854A (en) * | 2014-06-05 | 2014-08-13 | 深圳明阳电路科技有限公司 | Novel conductive adhesive and preparation method thereof |
| CN105860906A (en) * | 2016-06-21 | 2016-08-17 | 李康 | Conductive adhesive for LED (light-emitting diode) chip bonding |
| CN110136863A (en) * | 2019-04-29 | 2019-08-16 | 南通天盛新能源股份有限公司 | A kind of low-temperature conductive silver paste and preparation method thereof for HIT solar battery |
| CN113372844A (en) * | 2021-06-08 | 2021-09-10 | 北京中天鹏宇科技发展有限公司 | High-temperature-resistant epoxy resin conductive adhesive and preparation method thereof |
-
2022
- 2022-12-30 CN CN202211742124.8A patent/CN116130143A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302413A (en) * | 2008-07-01 | 2008-11-12 | 上海上大瑞沪微系统集成技术有限公司 | High temperature resistant epoxide resin conductive adhesive |
| CN103980854A (en) * | 2014-06-05 | 2014-08-13 | 深圳明阳电路科技有限公司 | Novel conductive adhesive and preparation method thereof |
| CN105860906A (en) * | 2016-06-21 | 2016-08-17 | 李康 | Conductive adhesive for LED (light-emitting diode) chip bonding |
| CN110136863A (en) * | 2019-04-29 | 2019-08-16 | 南通天盛新能源股份有限公司 | A kind of low-temperature conductive silver paste and preparation method thereof for HIT solar battery |
| CN113372844A (en) * | 2021-06-08 | 2021-09-10 | 北京中天鹏宇科技发展有限公司 | High-temperature-resistant epoxy resin conductive adhesive and preparation method thereof |
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