CN103666319A - Marine climate resistant epoxy conductive adhesive composition - Google Patents
Marine climate resistant epoxy conductive adhesive composition Download PDFInfo
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- CN103666319A CN103666319A CN201310672275.5A CN201310672275A CN103666319A CN 103666319 A CN103666319 A CN 103666319A CN 201310672275 A CN201310672275 A CN 201310672275A CN 103666319 A CN103666319 A CN 103666319A
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Abstract
The invention discloses a marine climate resistant epoxy conductive adhesive composition and a preparation method thereof. The composition comprises the following raw materials by weight percent: 40-50% of conductive silver powder, 5-10% of nano copper powder, 5-10% of carbon nanotubes, 10-25% of epoxy resin, 3-10% of dispersing agent, 8-20% of curing agent and 0.5-2% of curing accelerator. The conductive adhesive composition has the positive effects that the conductivity of the composition is greatly improved by adding the micron silver powder, nano copper powder and carbon nanotubes; the conductivity and thermal conductivity of the composition are simultaneously improved by adding the conductive and thermally conductive carbon nanotubes; meanwhile, the cost of the composition is greatly reduced by using the micron silver powder, nano copper powder and carbon nanotubes to replace part of the nano silver powder.
Description
Technical field
The present invention relates to a kind of epoxy conductive adhesive composition of marine climate resistant, be specifically related to a kind of epoxy conductive adhesive composition that adopts hybrid conductive powder and preparation method thereof.
Background technology
Conductive resin be a kind of solidify or dry after there is the sizing agent of certain conductivity, it take matrix resin and conductive filler material is conventionally that conducting particles is chief component composition, bonding effect by matrix resin combines conducting particles, form conductive path, realize by the conduction of sticky material and connecting.Because the matrix resin of conductive resin is a kind of sizing agent, can select suitable solidification value to carry out bonding, simultaneously, the densification of miniaturization, microminiaturization and printed circuit board (PCB) and developing rapidly of Highgrade integration due to electronic component, and conductive resin can be made slurry, realize very high linear resolution.And conductive resin technique is simple, easy handling, can enhance productivity, so conductive resin is to substitute slicker solder welding, realizes the ideal chose that conduction connects.
In the conductive resin field of marine climate resistant, epoxy resin is because its good performance is very extensive in the application in conductive resin field.But also there are some problems in epoxy resin binder system, such as viscosity is large, thermotolerance is lower, fragility is strong, the shelf time is short etc.Therefore develop a kind of modest viscosity, toughness is strong, high temperature resistant, and long epoxy conducting of shelf time becomes technical problem urgently to be resolved hurrily at present.
Meanwhile, conductive resin is mostly used silver powder as the filler with conduction and heat conductivility, and the major portion of its material cost is also silver powder.But along with industry member is day by day vigorous for the demand of the precious metal of silver etc., silver powder price is always constantly soaring, cause conductive resin shared cost in Electronic Packaging to rise significantly, so develop active demand that the conductive resin of a class lower cost meets market, become the problem that scientific circles and industry member are all concerned about very much.
Summary of the invention
For addressing the above problem, the invention provides a kind of epoxy conductive adhesive composition of marine climate resistant, thereby reach modest viscosity, toughness is strong, high temperature resistant, cost is low object.
An epoxy conductive adhesive composition for marine climate resistant, comprises each raw material of following weight percent: conductive silver powder 40%-50%, nano level copper powder 5-10%, CNT (carbon nano-tube) 5-10%, epoxy resin 10%-25%, dispersion agent 3%-10%, solidifying agent 8%-20%, curing catalyst 0.5%-2%.
Further, described conductive silver powder is nano-silver powder and micro-silver powder, and the mass ratio of nano-silver powder and micro-silver powder is 8:2.
Further, the particle diameter of described nano-silver powder is 20 nanometer-30 nanometers, and the particle diameter of described micro-silver powder is 5 microns-30 microns, and the particle diameter of copper nanoparticle is 50 nanometer-80 nanometers, and the particle diameter of described micron carbon pipe is 50 nanometer-80 nanometers.
Further, described epoxy resin is the one or any two or more mixture in glycolylurea epoxide resin, two Resorcinol acetal four glycidyl ethers, amino tetrafunctional epoxy resin, two (2,3-epoxy group(ing) cyclopentyl) ether.
Further, described dispersion agent is silane coupling agent, is the one or any two or more mixture in γ-aminopropyl methyldiethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or γ-aminopropyl triethoxysilane;
Further, described solidifying agent is that diaminodiphenylmethane and mphenylenediamine be take the mixture that mass ratio coordinates as 2:3.
Further, described curing catalyst is one or more the mixture in 2-benzyl-4-methylimidazole, 2-heptadecyl imidazoles, 2-undecyl imidazole, 2-ethyl-4-methylimidazole.
The invention also discloses a kind of preparation method of epoxy conductive adhesive composition of marine climate resistant: comprise the following steps:
1), by conductive silver powder, CNT (carbon nano-tube) mixes at 45-65 ℃, obtains its mixture, standby;
2) solidifying agent, curing catalyst and dispersion agent are joined in epoxy resin, and at room temperature mix, obtain mixture, then described mixture is put on shredder, and at room temperature grind 20 minutes, obtain a homogeneous mixture;
3) by obtaining mixture in step 1), join step 2) in the uniform mixture that makes, then add nano level copper powder, and at room temperature stir, to mixing, obtain described conducting resin composition.
Positively effect of the present invention is: add micro-silver powder, copper nanoparticle and CNT (carbon nano-tube) greatly to improve its conductivity, and add conduction and heat conducting nano carbon pipe more to improve its conduction and heat conductivility simultaneously, by micro-silver powder, copper nanoparticle and CNT (carbon nano-tube), replace part nano-silver powder simultaneously, greatly reduce its cost.
Embodiment
Below in conjunction with embodiment, describe technical scheme of the present invention in detail, but protection domain is not so limited.
100 grams of the epoxy conductive adhesive compositions of 1 one kinds of marine climate resistants of embodiment, each raw material that comprises following weight percent: 20 nano-silver powders 32%, 5 micro-silver powders 8%, nano level copper powder 10%, CNT (carbon nano-tube) 5%, glycolylurea epoxide resin 25%, γ-aminopropyl triethoxysilane 3%, ditane 6.6%, mphenylenediamine 9.9%, 2-heptadecyl imidazoles 0.5%.
A kind of preparation method of epoxy conductive adhesive composition of marine climate resistant: comprise the following steps:
1), by conductive silver powder, CNT (carbon nano-tube) mixes at 45 ℃, obtains its mixture, standby;
2) solidifying agent, curing catalyst and dispersion agent are joined in epoxy resin, and at room temperature mix, obtain mixture, then described mixture is put on shredder, and at room temperature grind 20 minutes, obtain a homogeneous mixture;
3) by obtaining mixture in step 1), join step 2) in the uniform mixture that makes, then add nano level copper powder, and at room temperature stir, to mixing, obtain described conducting resin composition.
The epoxy conductive adhesive composition of 2 one kinds of marine climate resistants of embodiment, each raw material that comprises following weight percent: 30 nano-silver powders 40%, 5 micro-silver powders 10%, nano level copper powder 5%, CNT (carbon nano-tube) 5%, two Resorcinol acetal four glycidyl ethers 7%, amino tetrafunctional epoxy resin 8%, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane 4%, γ-aminopropyl triethoxysilane 1%, diaminodiphenylmethane 7.6%, mphenylenediamine 11.4%, 2-heptadecyl imidazoles 1%.
The preparation method of the epoxy conductive adhesive composition of marine climate resistant: comprise the following steps:
1), by conductive silver powder, CNT (carbon nano-tube) mixes at 50 ℃, obtains its mixture, standby;
2) solidifying agent, curing catalyst and dispersion agent are joined in epoxy resin, and at room temperature mix, obtain mixture, then described mixture is put on shredder, and at room temperature grind 20 minutes, obtain a homogeneous mixture;
3) by obtaining mixture in step 1), join step 2) in the uniform mixture that makes, then add nano level copper powder, and at room temperature stir, to mixing, obtain described conducting resin composition.
The epoxy conductive adhesive composition of 3 one kinds of marine climate resistants of embodiment, each raw material that comprises following weight percent: nano-silver powder 36%, micro-silver powder 9%, nano level copper powder 8%, CNT (carbon nano-tube) 8%, amino tetrafunctional epoxy resin 15%, γ-aminopropyl methyldiethoxysilane 10%, diaminodiphenylmethane 4.8%, mphenylenediamine 7.2%, 2-benzyl-4-methylimidazole 2%.
The preparation method of the epoxy conductive adhesive composition of marine climate resistant: comprise the following steps:
1), by conductive silver powder, CNT (carbon nano-tube) mixes at 45-65 ℃, obtains its mixture, standby;
2) solidifying agent, curing catalyst and dispersion agent are joined in epoxy resin, and at room temperature mix, obtain mixture, then described mixture is put on shredder, and at room temperature grind 20 minutes, obtain a homogeneous mixture;
3) by obtaining mixture in step 1), join step 2) in the uniform mixture that makes, then add nano level copper powder, and at room temperature stir, to mixing, obtain described conducting resin composition.
For confirmatory experiment effect, the conducting resin composition of the marine climate resistant of above-described embodiment has been carried out to marine conductive and heat-conductive rate test:
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Electric conductivity (* 10 -4Ω·cm) | 25 | 30 | 20 |
| Thermal conductivity (W/mK) | 3.0 | 1.5 | 2.6 |
Due to visible, the conducting resin composition being designed by the present invention, is applicable to oceanographic engineering and uses, and has also kept good electrical and thermal conductivity performance when having reduced cost.
Claims (8)
1. the epoxy conductive adhesive composition of a marine climate resistant, it is characterized in that: each raw material that comprises following weight percent: conductive silver powder 40%-50%, nano level copper powder 5-10%, CNT (carbon nano-tube) 5-10%, epoxy resin 10%-25%, dispersion agent 3%-10%, solidifying agent 8%-20%, curing catalyst 0.5%-2%.
2. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 1, it is characterized in that, described conductive silver powder is nano-silver powder and micro-silver powder, and the mass ratio of nano-silver powder and micro-silver powder is 8:2.
3. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 2, it is characterized in that, the particle diameter of described nano-silver powder is 20 nanometer-30 nanometers, the particle diameter of described micro-silver powder is 5 microns-30 microns, the particle diameter of copper nanoparticle is 50 nanometer-80 nanometers, and the particle diameter of described micron carbon pipe is 50 nanometer-80 nanometers.
4. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 1, it is characterized in that, described epoxy resin is the one or any two or more mixture in glycolylurea epoxide resin, two Resorcinol acetal four glycidyl ethers, amino tetrafunctional epoxy resin, two (2,3-epoxy group(ing) cyclopentyl) ether.
5. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 1, it is characterized in that, described dispersion agent is silane coupling agent, for the one or any two or more mixture in γ-aminopropyl methyldiethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or γ-aminopropyl triethoxysilane.
6. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 1, it is characterized in that, described solidifying agent is that diaminodiphenylmethane and mphenylenediamine be take the mixture that mass ratio coordinates as 2:3.
7. according to the epoxy conductive adhesive composition of a kind of marine climate resistant described in claim 1, it is characterized in that, described curing catalyst is one or more the mixture in 2-benzyl-4-methylimidazole, 2-heptadecyl imidazoles, 2-undecyl imidazole, 2-ethyl-4-methylimidazole.
8. a preparation method for the epoxy conductive adhesive composition of marine climate resistant, is characterized in that, comprises the following steps:
1), by conductive silver powder, CNT (carbon nano-tube) mixes at 45-65 ℃, obtains its mixture, standby;
2) solidifying agent, curing catalyst and dispersion agent are joined in epoxy resin, and at room temperature mix, obtain mixture, then described mixture is put on shredder, and at room temperature grind 20 minutes, obtain a homogeneous mixture;
3) by obtaining mixture in step 1), join step 2) in the uniform mixture that makes, then add nano level copper powder, and at room temperature stir, to mixing, obtain described conducting resin composition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310672275.5A CN103666319B (en) | 2013-12-11 | 2013-12-11 | A kind of epoxy conductive adhesive composition of marine climate resistant |
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| CN201310672275.5A CN103666319B (en) | 2013-12-11 | 2013-12-11 | A kind of epoxy conductive adhesive composition of marine climate resistant |
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| CN103666319B CN103666319B (en) | 2016-04-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
| CN108913071A (en) * | 2018-05-02 | 2018-11-30 | 苏州耐思特塑胶有限公司 | A kind of conductive adhesive of anti-aging stability |
| CN114334222A (en) * | 2022-01-13 | 2022-04-12 | 深圳市普瑞威科技有限公司 | Conductive silver paste for relay contact and preparation method thereof |
| CN114512261A (en) * | 2022-03-29 | 2022-05-17 | 衡阳思迈科科技有限公司 | Low-temperature curing conductive silver paste and preparation method thereof |
| CN115058203A (en) * | 2022-07-27 | 2022-09-16 | 常州宏巨电子科技有限公司 | Formula and preparation method of micro-nano hybrid thermosetting conductive adhesive film |
Citations (2)
| 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 |
| CN103351836A (en) * | 2013-07-04 | 2013-10-16 | 张立强 | COB (Chip on Board) heat conduction adhesive |
-
2013
- 2013-12-11 CN CN201310672275.5A patent/CN103666319B/en active Active
Patent Citations (2)
| 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 |
| CN103351836A (en) * | 2013-07-04 | 2013-10-16 | 张立强 | COB (Chip on Board) heat conduction adhesive |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
| CN108913071A (en) * | 2018-05-02 | 2018-11-30 | 苏州耐思特塑胶有限公司 | A kind of conductive adhesive of anti-aging stability |
| CN114334222A (en) * | 2022-01-13 | 2022-04-12 | 深圳市普瑞威科技有限公司 | Conductive silver paste for relay contact and preparation method thereof |
| CN114334222B (en) * | 2022-01-13 | 2024-07-12 | 深圳市普瑞威科技有限公司 | Conductive silver paste for relay contacts and preparation method thereof |
| CN114512261A (en) * | 2022-03-29 | 2022-05-17 | 衡阳思迈科科技有限公司 | Low-temperature curing conductive silver paste and preparation method thereof |
| CN114512261B (en) * | 2022-03-29 | 2024-04-16 | 衡阳思迈科科技有限公司 | Low-temperature curing conductive silver paste and preparation method thereof |
| CN115058203A (en) * | 2022-07-27 | 2022-09-16 | 常州宏巨电子科技有限公司 | Formula and preparation method of micro-nano hybrid thermosetting conductive adhesive film |
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| CN103666319B (en) | 2016-04-06 |
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Address after: 266000 Qingdao science and technology, Huangdao District, Shandong, No. two road, No. 167 Patentee after: Qingdao Advanced Marine Material Technology Co., Ltd. Address before: 266101, Qingdao Road, Zhuzhou District, Shandong, Laoshan, 143 Patentee before: Qingdao Advanced Marine Material Technology Co., Ltd. |
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