CN1632032A - Monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive - Google Patents
Monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive Download PDFInfo
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- CN1632032A CN1632032A CN 200410068197 CN200410068197A CN1632032A CN 1632032 A CN1632032 A CN 1632032A CN 200410068197 CN200410068197 CN 200410068197 CN 200410068197 A CN200410068197 A CN 200410068197A CN 1632032 A CN1632032 A CN 1632032A
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Abstract
The invention relates to a flexible epoxide conducting silver glue with single component and can be solidified in the indoor temperature. In the usual temperature, mix 100 portions of bisphenol an epoxide resin whose epoxide equivalent is 200-250,5-30 portions of polyepoxide group epoxide resin whose epoxide equivalent is 120-150,50-800 portions of sticker,50-500 portions of alcohol averagely,the add into 450-3500 portions of slice-shaped silver powder whose average size is 1-10mm. In the indoor temperature,the invention can be solidified into the product with adhering strength and outstanding flexibility.
Description
Technical field
What the present invention relates to is a kind of conductive resin, and particularly a kind of single component and flexible and elastic epoxy conductive silver adhesive that can self-vulcanizing belong to the new function material field.
Background technology
Conductive resin is used widely in industries such as electronics, information, is mainly used in the conductive adhesive between the object.Because in many occasions, product will experience a shock, so conductive resin can experience a shock to the firm degree of object agglutinating, has become the major issue that application person is concerned about.Under such background condition, the good gentle elastic conduction glue of shock resistance arises at the historic moment.
The gentle elasticity of conductive resin is decided by the matrix resin of conductive resin.Usually adopt Resins, epoxy or urethane matrix resin as conductive resin.In Resins, epoxy, add flexible macromole such as rubber, adopt the flexible amine of long-chain can improve the original fragility of Resins, epoxy, thereby make Resins, epoxy show good gentle elasticity as methods such as solidifying agent.Urethane then itself just can obtain good gentle elasticity by the kind and the ratio of regulating component.
United States Patent (USP) 5891367 has been reported a kind of preparation method of epoxy conducting.Its adopt epoxy equivalent (weight) value at the bisphenol A type epoxy resin of 170-280 scope as resin matrix, the ether amine that adopts different chain length is as solidifying agent, adopt the conductive metal powder as conductive filler material, mix the back and obtain having good gentle elastic conductive articles 100-140 degree centigrade of curing.Adopt ether amine as the advantage of epoxy curing agent be can be easily the quantity of length by regulating ether amine and amidine functional group control soft degree after the adhesive curing.But insufficient is that cohesive strength and flexibility after this adhesive curing conditions each other, and obtain higher bonding strength, just must sacrifice the flexibility of cured product.The cohesive strength of the conductive resin that this individual system obtains generally is lower than 5MPa, and for some Application Areass that cohesive strength is had relatively high expectations, it is inapplicable.
On the other hand, present flexible epoxy conductive resin all requires to be cured under comparatively high temps, at room temperature can deposit the long period simultaneously.But in a lot of occasions, because by the restriction of bonding object or operating procedure condition, conductive resin can not be heating and curing, and can only ambient cure.Therefore, be necessary very much to develop high comprehensive performance, and single component flexible and elastic epoxy conductive glue that can ambient cure.
Put it briefly, the cohesive strength of the gentle elastic conduction glue of prior art and room temp solidified not ideal enough has much room for improvement.
Summary of the invention
The object of the present invention is to provide a kind of flexible and elastic epoxy conductive silver adhesive of single component ambient temperature curable, this conductive resin is easy to use, and it is promptly curable to need not heating, and has good impact resistance and extraordinary adhesive property.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals: the making method of monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive, it is characterized in that: at normal temperatures, with weight ratio 100 parts the bisphenol A epoxide resin of epoxy equivalent (weight) in the 200-250 scope, the many epoxide group Resins, epoxy of 5-30 part epoxy equivalent (weight) in the 120-150 scope, 50-800 part solidifying agent, after 50-500 part ethanol thorough mixing is even, adding 450-3500 part mean sizes is the flake silver powder of 1-10 micron, further thorough mixing.This conductive resin can be solidified into the product of gentle excellent spring in 24 hours under 25 degrees centigrade room temperature environment.
In the epoxy resin system conductive of prior art, the Resins, epoxy that is adopted mostly is bisphenol A epoxide resin, and its epoxy equivalent (weight) scope is generally at 170-280, and does not have to adopt the Resins, epoxy of low epoxy equivalent (weight).The present invention is that bisphenol A epoxide resin and epoxy equivalent (weight) in the 200-250 scope is that many epoxide groups Resins, epoxy of 120-150 mixes use with epoxy equivalent (weight), in this mixed system, epoxy equivalent (weight) is the effect that many epoxide groups Resins, epoxy of 120-150 plays raising system cohesive strength and reduction resin system viscosity simultaneously, is a kind of very special and crucial resin matrix.
The present invention adopts dehydrated alcohol as thinner, reduces the viscosity of system, the shelf time of improving conductive resin simultaneously.
Technical scheme of the present invention can also be further perfect, as preferably, add the curing catalyst DMP-30 of weight ratio 0.1-6 part before adding silver powder, and thorough mixing is even.
Curing catalyst DMP-30 promptly 2,4,6-three-(dimethylamino methyl)-phenol, in low molecular polyamides and fatty ether amine hardener, can use, wherein in fatty ether amine hardener system, use DMP-30 not appear in the newspapers.The curing speed of general fatty ether amine hardener is slow, by adding DMP-30, can obviously improve the curing speed of system.
As preferably, described solidifying agent is low molecular polyamides and/or fatty ether amine.
Solidifying agent in the invention can be that low molecular polyamides or fatty ether amine use separately separately, also can be that low molecular polyamides and fatty ether amine use jointly.Under the situation of simple employing low molecular polyamides, resulting cured product snappiness is better, but does not have elasticity.Under the situation of simple employing aliphatic polyether amine, though resulting cured product has gentle preferably elasticity, intensity and toughness are relatively poor.By two kinds of solidifying agent of compound employing, the existing gentle preferably elasticity of the cured product that obtains has intensity and toughness preferably again.The method of this compound employing low molecular polyamides and fatty ether amine hardener is a first Application of the present invention, and the molecular weight ranges of the low molecular polyamides that is adopted is at 150-1000.
The fatty ether amine hardener that the present invention uses is the binary or the ternary aliphatic family ether amine of different chain length.Its molecular weight ranges is recommended as 2000 at 400-5000.
The present invention has following characteristics and advantage:
1. the present invention has adopted the epoxy-resin systems of high epoxy equivalent (weight) and low epoxy equivalent (weight) blend, and low epoxy equivalent (weight) resin wherein is many epoxide groups Resins, epoxy;
2. in the single-component epoxy system, adopt low molecular polyamides as introducing gentle elastic solidifying agent;
3. the epoxy conductive silver glue that obtains of invention fast setting at room temperature has good self-vulcanizing performance;
4. invent the flexible epoxy conductive resin that obtains and have superior bond strengths rendering, its cohesive strength is the highest can be higher than 10MPa.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described in detail:
Embodiment one:
With epoxy equivalent (weight) is 100 parts of 200 bisphenol A epoxide resins, with 5 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 120 mixes, the molecular weight that adds 50 parts then is 150 low molecular polyamides, continue to mix, add 50 parts of ethanol again, 200 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the snappiness product in 18 hours under 25 degrees centigrade room temperature environment, elasticity is relatively poor, and its volume specific resistance is 9 * 10
-4Ohmcm, cohesive strength are 10.5MPa.
Embodiment two:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 30 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, add 600 parts of molecular weight then and be 2000 dibasic aliphatic ether amine, continue to mix, add 300 parts of ethanol again, 2190 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the product of gentle excellent spring in 24 hours, but toughness is relatively poor under 25 degrees centigrade room temperature environment, its volume specific resistance is 2.4 * 10
-4Ohmcm, cohesive strength are 2.2MPa.
Embodiment three:
With epoxy equivalent (weight) is 100 parts of 200 bisphenol A epoxide resins, with 30 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 120 mixes, the molecular weight that adds 800 parts then is 2000 dibasic aliphatic ether amine, continue to mix, add 3 parts of 500 parts of ethanol and DMP-30 again, 3500 parts of mean sizess of adding are 10 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the product of gentle excellent spring in 12 hours under 25 degrees centigrade room temperature environment, toughness is relatively poor, and its volume specific resistance is 4.2 * 10
-5Ohmcm, cohesive strength are 3.8MPa.
Embodiment four:
With epoxy equivalent (weight) is 100 parts of 220 bisphenol A epoxide resins, with 15 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 130 mixes, add 70 parts of molecular weight then and be 1000 low molecular polyamides, continue to mix, add 6 parts of 150 parts of ethanol and DMP-30 again, 450 parts of mean sizess of adding are 7 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the good product of snappiness in 6 hours under 25 degrees centigrade room temperature environment, elasticity is relatively poor, and its volume specific resistance is 1.1 * 10
-4Ohmcm, cohesive strength are 9.4MPa.
Embodiment five:
With epoxy equivalent (weight) is 100 parts of 200 bisphenol A epoxide resins, with 5 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 120 mixes, the molecular weight that adds 50 parts then is 800 low molecular polyamides, continue to mix, add 50 parts of ethanol again, 200 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the snappiness product in 18 hours under 25 degrees centigrade room temperature environment, elasticity is relatively poor, and its volume specific resistance is 9 * 10
-4Ohmcm, cohesive strength are 12.0MPa.
Embodiment six:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 20 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 120 mixes, the molecular weight that adds 60 parts then is 1000 low molecular polyamides, continue to mix, add 50 parts of ethanol again, 665 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the snappiness product in 12 hours under 25 degrees centigrade room temperature environment, elasticity is relatively poor, and its volume specific resistance is 3.6 * 10
-4Ohmcm, cohesive strength are 7.8MPa.
Embodiment seven:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 5 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, the molecular weight that adds 250 parts then is that 5000 dibasic aliphatic ether amine and 40 parts of molecular weight are 403 ternary aliphatic family ether amine, continue to mix, add 50 parts of ethanol again, 875 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into gentle elasticity product in 12 hours under 25 degrees centigrade room temperature environment, toughness is relatively poor, and its volume specific resistance is 1.8 * 10
-4Ohmcm, cohesive strength are 8.5MPa.
Embodiment eight:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 5 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, the molecular weight that adds 80 parts then is 1000 low molecular polyamides, continue to mix, add 3 parts of 50 parts of ethanol and DMP-30 again, 430 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the snappiness product in 6 hours under 25 degrees centigrade room temperature environment, elasticity is relatively poor, and its volume specific resistance is 2.3 * 10
-4Ohmcm, cohesive strength are 13.4MPa.
Embodiment nine:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 30 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, add 600 parts of molecular weight then and be 2000 dibasic aliphatic ether amine, continue to mix, add 300 parts of ethanol and 6 parts of DMP-30 again, 2190 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into the product of gentle excellent spring in 8 hours under 25 degrees centigrade room temperature environment, toughness is relatively poor, and its volume specific resistance is 3.4 * 10
-4Ohmcm, cohesive strength are 3.3MPa.
Embodiment ten:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 30 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, add 600 parts of molecular weight then and be 2000 dibasic aliphatic ether amine, continue to mix, add molecular weight again and be 30 parts of 500 low molecular polyamides, add 300 parts of ethanol and 6 parts of DMP-30 again, 3200 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into gentle elasticity and all excellent product of toughness in 5 hours under 25 degrees centigrade room temperature environment, its volume specific resistance is 3.8 * 10
-4Ohmcm, cohesive strength are 7.5MPa.
Embodiment 11:
With epoxy equivalent (weight) is 100 parts of 250 bisphenol A epoxide resins, with 30 parts of epoxy equivalent (weight)s be that many epoxide groups Resins, epoxy of 150 mixes, add 120 parts of molecular weight then and be 400 dibasic aliphatic ether amine, continue to mix, add molecular weight again and be 20 parts of 1000 low molecular polyamides, add 300 parts of ethanol and 3 parts of DMP-30 again, 630 parts of mean sizess of adding are 5 microns flake silver powder after mixing, and obtain conductive resin after further thorough mixing is even.This conductive resin can be solidified into gentle elasticity and all excellent product of toughness in 6 hours under 25 degrees centigrade room temperature environment, its volume specific resistance is 2.8 * 10
-4Ohmcm, cohesive strength are 11.2MPa.
Claims (3)
1, a kind of monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive, it is characterized in that: at normal temperatures, with weight ratio 100 parts the bisphenol A epoxide resin of epoxy equivalent (weight) in the 200-250 scope, the many epoxide group Resins, epoxy of 5-30 part epoxy equivalent (weight) in the 120-150 scope, 50-800 part solidifying agent, after 50-500 part ethanol thorough mixing was even, adding 450-3500 part mean sizes was the flake silver powder of 1-10 micron, further thorough mixing.
2, monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive according to claim 1 is characterized in that: add the curing catalyst DMP-30 of weight ratio 0.1-6 part before adding silver powder, and thorough mixing is even.
3, monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive according to claim 1 and 2 is characterized in that: described solidifying agent is low molecular polyamides and/or fatty ether amine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410068197 CN1247729C (en) | 2004-11-11 | 2004-11-11 | Monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410068197 CN1247729C (en) | 2004-11-11 | 2004-11-11 | Monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive |
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| CN1632032A true CN1632032A (en) | 2005-06-29 |
| CN1247729C CN1247729C (en) | 2006-03-29 |
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| CN 200410068197 Expired - Fee Related CN1247729C (en) | 2004-11-11 | 2004-11-11 | Monocomponent room-temperature cured flexible and elastic epoxy conductive silver adhesive |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101818037A (en) * | 2009-02-27 | 2010-09-01 | 汉高（中国）投资有限公司 | Room-temperature curing epoxy structural adhesive composition and preparation method thereof |
| CN101245227B (en) * | 2007-02-13 | 2010-09-08 | 核工业第八研究所 | Epoxy conductive silver glue for LED and method for manufacturing same |
| CN101148571B (en) * | 2007-10-19 | 2010-10-06 | 东华大学 | Fire resistant epoxy conducting adhesive and preparation method thereof |
| CN102040916A (en) * | 2009-10-23 | 2011-05-04 | 比亚迪股份有限公司 | Silver conductive adhesive as well as preparation method and application thereof |
| CN102040934A (en) * | 2009-10-23 | 2011-05-04 | 比亚迪股份有限公司 | Silver conductive adhesive and preparation method thereof |
| CN102101988A (en) * | 2010-12-29 | 2011-06-22 | 河南农业大学 | Conductive elargol for use in pest electrical penetration graph technology |
| CN102922213A (en) * | 2012-11-21 | 2013-02-13 | 苏州永创金属科技有限公司 | Method for repairing surface defect of silver-plated workpiece at low temperature without color difference |
| CN105646968A (en) * | 2016-03-02 | 2016-06-08 | 安徽汇精模具研发科技有限公司 | Denoising electroconductive rubber gasket |
| RU2612717C2 (en) * | 2015-06-23 | 2017-03-13 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Томский государственный университет систем управления и радиоэлектроники" | Current-conducting adhesive composition |
| CN106684404A (en) * | 2017-01-05 | 2017-05-17 | 北京氢璞创能科技有限公司 | Fuel cell controller package design |
| RU2662513C1 (en) * | 2017-10-05 | 2018-07-26 | Акционерное общество "Научно-производственное предприятие "Исток" имени А.И. Шокина" (АО "НПП "Исток" им. Шокина") | Adhesive composition for electronic microwave technology |
| CN110330926A (en) * | 2019-07-11 | 2019-10-15 | 上海闰龙电子材料有限公司 | A kind of high-bond high thermal conductivity fire retarding epoxide resin adhesive and preparation method thereof |
| US11629455B2 (en) | 2020-04-22 | 2023-04-18 | Taiwan Textile Research Institute | Conductive textile and method for fabricating the same |
| CN117487492A (en) * | 2023-12-15 | 2024-02-02 | 深圳宏鑫新材料科技有限公司 | Room temperature curing conductive adhesive and preparation method thereof |
-
2004
- 2004-11-11 CN CN 200410068197 patent/CN1247729C/en not_active Expired - Fee Related
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| CN101245227B (en) * | 2007-02-13 | 2010-09-08 | 核工业第八研究所 | Epoxy conductive silver glue for LED and method for manufacturing same |
| CN101148571B (en) * | 2007-10-19 | 2010-10-06 | 东华大学 | Fire resistant epoxy conducting adhesive and preparation method thereof |
| CN101818037A (en) * | 2009-02-27 | 2010-09-01 | 汉高（中国）投资有限公司 | Room-temperature curing epoxy structural adhesive composition and preparation method thereof |
| CN101818037B (en) * | 2009-02-27 | 2014-12-31 | 汉高（中国）投资有限公司 | Room-temperature curing epoxy structural adhesive composition and preparation method thereof |
| CN102040916B (en) * | 2009-10-23 | 2013-06-19 | 比亚迪股份有限公司 | Silver conductive adhesive as well as preparation method and application thereof |
| CN102040934A (en) * | 2009-10-23 | 2011-05-04 | 比亚迪股份有限公司 | Silver conductive adhesive and preparation method thereof |
| CN102040916A (en) * | 2009-10-23 | 2011-05-04 | 比亚迪股份有限公司 | Silver conductive adhesive as well as preparation method and application thereof |
| CN102101988B (en) * | 2010-12-29 | 2012-08-22 | 河南农业大学 | Conductive elargol for use in pest electrical penetration graph technology |
| CN102101988A (en) * | 2010-12-29 | 2011-06-22 | 河南农业大学 | Conductive elargol for use in pest electrical penetration graph technology |
| CN102922213A (en) * | 2012-11-21 | 2013-02-13 | 苏州永创金属科技有限公司 | Method for repairing surface defect of silver-plated workpiece at low temperature without color difference |
| CN102922213B (en) * | 2012-11-21 | 2014-12-03 | 苏州永创金属科技有限公司 | Method for repairing surface defect of silver-plated workpiece at low temperature without color difference |
| RU2612717C2 (en) * | 2015-06-23 | 2017-03-13 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Томский государственный университет систем управления и радиоэлектроники" | Current-conducting adhesive composition |
| CN105646968A (en) * | 2016-03-02 | 2016-06-08 | 安徽汇精模具研发科技有限公司 | Denoising electroconductive rubber gasket |
| CN106684404A (en) * | 2017-01-05 | 2017-05-17 | 北京氢璞创能科技有限公司 | Fuel cell controller package design |
| RU2662513C1 (en) * | 2017-10-05 | 2018-07-26 | Акционерное общество "Научно-производственное предприятие "Исток" имени А.И. Шокина" (АО "НПП "Исток" им. Шокина") | Adhesive composition for electronic microwave technology |
| CN110330926A (en) * | 2019-07-11 | 2019-10-15 | 上海闰龙电子材料有限公司 | A kind of high-bond high thermal conductivity fire retarding epoxide resin adhesive and preparation method thereof |
| US11629455B2 (en) | 2020-04-22 | 2023-04-18 | Taiwan Textile Research Institute | Conductive textile and method for fabricating the same |
| CN117487492A (en) * | 2023-12-15 | 2024-02-02 | 深圳宏鑫新材料科技有限公司 | Room temperature curing conductive adhesive and preparation method thereof |
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| CN1247729C (en) | 2006-03-29 |
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