CN102443372A - Electron beam solidified epoxy resin conductive adhesive and preparation method thereof - Google Patents
Electron beam solidified epoxy resin conductive adhesive and preparation method thereof Download PDFInfo
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- CN102443372A CN102443372A CN2011103241010A CN201110324101A CN102443372A CN 102443372 A CN102443372 A CN 102443372A CN 2011103241010 A CN2011103241010 A CN 2011103241010A CN 201110324101 A CN201110324101 A CN 201110324101A CN 102443372 A CN102443372 A CN 102443372A
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- epoxy resin
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- conductive filler
- electrocuring
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Abstract
The invention discloses an electron beam solidified epoxy resin conductive adhesive and a preparation method thereof. The method comprises steps of: dispersing a conductive filling material in acetone and adding bisphenol A epoxy resin and mixing well the resin and the conductive filling material; then adding an electron beam curing agent, stirring to dissolve and well mixing the electron beam curing agent with the conductive filling material and the epoxy resin; finally carrying out atmospheric distillation at 60-80 DEG C, removing the solvent and carrying out vacuum drying under 60 DEG C for 2h to obtain the electron beam solidified epoxy resin conductive adhesive. The electron beam solidified epoxy resin conductive adhesive provided by the invention comprises epoxy resin, conductive filling material and electron beam curing agent, has low toxicity and little pollution and can be stored under room temperature for a long time. According to electron beam irradiation, the electron beam solidified epoxy resin conductive adhesive can solidify under a room temperature or a low temperature in few minutes and has high bonding strength and conductivity.
Description
Technical field
The invention belongs to novel high polymer composite conducting technical field of adhesive, more particularly, relate to a kind of electron beam curing of epoxy resins electroconductive binder and preparation method thereof.
Background technology
Electroconductive binder is to glued joint the tackiness agent that various materials have conductivity again.The composite conducting tackiness agent is that to add with synthetic resins be matrix, adds electroconductive stuffings such as metal-powder, graphitized carbon black or carbon nanotube, has the tackiness agent of electric action after the curing.Field such as electro-conductive adhesive is widely used in microelectronics Packaging, electronic devices and components are bonding, transmitter is connected with battery electrode and the Electronic Micro-Analysis sample is bonding.
The epoxies tackiness agent is widely used in fields such as Aeronautics and Astronautics, machinery, electronics because bonding strength is high, highly versatile.Yet general epoxies tackiness agent is made up of epoxy resin and solidifying agent, and it is short that each component is mixed back storage period, and the curing of seriously polluted during use, tackiness agent need be carried out under long period or higher temperature.
Electrocuring is to utilize electron beam irradiation to treat curing material, and electron beam passes to medium molecule through the collision with medium with energy at short notice, produces chemical transformation, causes the resin crosslinks reaction and makes material cured.Electrocuring can carry out under room temperature or low temperature, and curing speed is far above thermofixation, and cured product meets or exceeds traditional thermofixation product at aspects such as mechanical property, water-intake rate, second-order transition temperatures.Electrocuring is used for epoxy resin and matrix material is very promising technology, has caused the attention of various countries research institution and decision-making section.
Summary of the invention
The objective of the invention is to overcome shortcomings such as common epoxies electroconductive binder storage period is short, solidification value is high, set time is long, utilize Electron beam curing technology, but epoxy resin conduction tackiness agent of a kind of electrocuring and preparation method thereof is provided.
A kind of electron beam curing of epoxy resins electroconductive binder prepares according to following step:
(1) conductive filler material is dispersed in the acetone, adds bisphenol A type epoxy resin, resin and conductive filler material are mixed;
(2) in step (1) gained mixed system, add the electrocuring agent, stirring makes it dissolving and mixes with conductive filler material and epoxy resin;
(3), remove acetone solvent in step (2) the gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring 60～80 ℃ of following air distillations.
In the said step (1), conductive filler material is silver powder, graphitized carbon black and carbon nanotube, and the mass ratio of conductive filler material and epoxy resin is 5～10: 100.
In the said step (2), the electrocuring agent is a diphenyl iodine hexafluorophosphate, and the mass ratio of diphenyl iodine hexafluorophosphate and epoxy resin is 2～5: 100.
A kind of preparation method of electron beam curing of epoxy resins electroconductive binder prepares according to following step:
(1) conductive filler material is dispersed in the acetone, adds bisphenol A type epoxy resin, resin and conductive filler material are mixed;
(2) in step (1) gained mixed system, add the electrocuring agent, stirring makes it dissolving and mixes with conductive filler material and epoxy resin;
(3), remove acetone solvent in step (2) the gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring 60～80 ℃ of following air distillations.
In the said step (1), conductive filler material is silver powder, graphitized carbon black and carbon nanotube, and the mass ratio of conductive filler material and epoxy resin is 5～10: 100.
In the said step (2), the electrocuring agent is a diphenyl iodine hexafluorophosphate, and the mass ratio of diphenyl iodine hexafluorophosphate and epoxy resin is 2～5: 100.
Electron beam curing of epoxy resins electroconductive binder provided by the present invention is made up of epoxy resin, conductive filler material and electrocuring agent, and toxicity is low, pollution is little, but prolonged storage at room temperature.Through electron beam irradiation, can under room temperature or low temperature, in several minutes, accomplish curing reaction, have higher bonding strength and electroconductibility.This electron beam curing of epoxy resins electroconductive binder has broad application prospects and higher utility in fields such as microelectronics Packaging, photoelectric component, transmitter, secondary cell and Electronic Micro-Analysis.
Embodiment
Below through specific embodiment technical scheme of the present invention is further described:
Embodiment 1
The first step is dispersed in 0.25 gram multi-walled carbon nano-tubes in 50 milliliters of acetone, adds 5 gram bisphenol A type epoxy resin E-44, and resin and conductive filler material are mixed.
Second step added 0.15 gram electrocuring agent diphenyl iodine hexafluorophosphate in step 1 gained mixed system, stir to make it to dissolve and mix with conductive filler material and epoxy resin.
In the 3rd step, 60～80 ℃ of following air distillations, remove acetone solvent in the step 2 gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring.
The gained tackiness agent is coated on the deckglass, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 300 seconds.Measure tackiness agent according to GB/T 15662 and solidify the back surface resistivity.
Tackiness agent is coated on the rigidity coupon splicing face, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 300 seconds.Measure tackiness agent opposite joint tensile strength according to GB-T-6329-1996.
The epoxy resin conduction tackiness agent test result of embodiment 1 gained ability electrocuring is seen table 1.
Embodiment 2
The first step is led carbon black with 0.5 gram height and is dispersed in 50 milliliters of acetone, adds 10 gram bisphenol A type epoxy resin E-44, and resin and conductive filler material are mixed.
Second step added 0.3 gram electrocuring agent diphenyl iodine hexafluorophosphate in step 1 gained mixed system, stir to make it to dissolve and mix with conductive filler material and epoxy resin.
In the 3rd step, 60～80 ℃ of following air distillations, remove acetone solvent in the step 2 gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring.
The gained tackiness agent is coated on the deckglass, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 600 seconds.Measure tackiness agent according to GB/T 15662 and solidify the back surface resistivity.
Tackiness agent is coated on the rigidity coupon splicing face, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 300 seconds.Measure tackiness agent opposite joint tensile strength according to GB-T-6329-1996.
The epoxy resin conduction tackiness agent test result of embodiment 2 gained ability electrocuring is seen table 1.
Embodiment 3
The first step is dispersed in 1.00 gram super fine silver powders in 50 milliliters of acetone, adds 10 gram bisphenol A type epoxy resin E-44, and resin and conductive filler material are mixed.
Second step added 0.5 gram electrocuring agent diphenyl iodine hexafluorophosphate in step 1 gained mixed system, stir to make it to dissolve and mix with conductive filler material and epoxy resin.
In the 3rd step, 60～80 ℃ of following air distillations, remove acetone solvent in the step 2 gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring.
The gained tackiness agent is coated on the deckglass, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 600 seconds.Measure tackiness agent according to GB/T 15662 and solidify the back surface resistivity.
Tackiness agent is coated on the rigidity coupon splicing face, uses linear electron accelerator irradiation, power 0.7kW, energy 5MeV, radiation dose rate 50Gy/s, irradiation be tackiness agent curing after 300 seconds.Measure tackiness agent opposite joint tensile strength according to GB-T-6329-1996.
The epoxy resin conduction tackiness agent test result of embodiment 3 gained ability electrocuring is seen table 1.
Table 1 is respectively implemented performance test data
Claims (6)
1. an electron beam curing of epoxy resins electroconductive binder is characterized in that, prepares according to following step:
(1) conductive filler material is dispersed in the acetone, adds bisphenol A type epoxy resin, resin and conductive filler material are mixed;
(2) in step (1) gained mixed system, add the electrocuring agent, stirring makes it dissolving and mixes with conductive filler material and epoxy resin;
(3), remove acetone solvent in step (2) the gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring 60～80 ℃ of following air distillations.
2. a kind of electron beam curing of epoxy resins electroconductive binder according to claim 1 is characterized in that, in the said step (1), conductive filler material is silver powder, graphitized carbon black and carbon nanotube, and the mass ratio of conductive filler material and epoxy resin is 5～10: 100.
3. a kind of electron beam curing of epoxy resins electroconductive binder according to claim 1; It is characterized in that; In the said step (2), the electrocuring agent is a diphenyl iodine hexafluorophosphate, and the mass ratio of diphenyl iodine hexafluorophosphate and epoxy resin is 2～5: 100.
4. the preparation method of an electron beam curing of epoxy resins electroconductive binder is characterized in that, prepares according to following step:
(1) conductive filler material is dispersed in the acetone, adds bisphenol A type epoxy resin, resin and conductive filler material are mixed;
(2) in step (1) gained mixed system, add the electrocuring agent, stirring makes it dissolving and mixes with conductive filler material and epoxy resin;
(3), remove acetone solvent in step (2) the gained mixture, and in 60 ℃ of following vacuum-dryings 2 hours, but obtain the epoxy resin conduction tackiness agent of electrocuring 60～80 ℃ of following air distillations.
5. the preparation method of a kind of electron beam curing of epoxy resins electroconductive binder according to claim 4; It is characterized in that; In the said step (1), conductive filler material is silver powder, graphitized carbon black and carbon nanotube, and the mass ratio of conductive filler material and epoxy resin is 5～10: 100.
6. the preparation method of a kind of electron beam curing of epoxy resins electroconductive binder according to claim 4; It is characterized in that; In the said step (2), the electrocuring agent is a diphenyl iodine hexafluorophosphate, and the mass ratio of diphenyl iodine hexafluorophosphate and epoxy resin is 2～5: 100.
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| CN2011103241010A CN102443372A (en) | 2011-10-21 | 2011-10-21 | Electron beam solidified epoxy resin conductive adhesive and preparation method thereof |
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| CN2011103241010A CN102443372A (en) | 2011-10-21 | 2011-10-21 | Electron beam solidified epoxy resin conductive adhesive and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903654A (en) * | 2017-11-22 | 2018-04-13 | 昆山创匠新材料科技有限公司 | A kind of resin combination and preparation method thereof |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
| CN113278388A (en) * | 2021-04-26 | 2021-08-20 | 青岛歌尔微电子研究院有限公司 | Conductive silver adhesive and preparation method thereof |
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| CN101033379A (en) * | 2006-03-10 | 2007-09-12 | 国家淀粉及化学投资控股公司 | Anisotropic conductive adhesive |
| JP2008127553A (en) * | 2006-11-24 | 2008-06-05 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing, and semiconductor device using it |
| CN101431145A (en) * | 2008-12-08 | 2009-05-13 | 电子科技大学 | Substrate for flexible organic opto-electronic device and method for producing the same |
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2011
- 2011-10-21 CN CN2011103241010A patent/CN102443372A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033379A (en) * | 2006-03-10 | 2007-09-12 | 国家淀粉及化学投资控股公司 | Anisotropic conductive adhesive |
| JP2008127553A (en) * | 2006-11-24 | 2008-06-05 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing, and semiconductor device using it |
| CN101431145A (en) * | 2008-12-08 | 2009-05-13 | 电子科技大学 | Substrate for flexible organic opto-electronic device and method for producing the same |
Non-Patent Citations (3)
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| 《高分子学报》 20020720 张佐光等 《电子束辐射固化环氧树脂的动态力学分析--树脂化学结构、分子量及其分布的影响 》 426-431 1-6 , 第4期 * |
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| 张佐光等: "《电子束辐射固化环氧树脂的动态力学分析——树脂化学结构、分子量及其分布的影响 》", 《高分子学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903654A (en) * | 2017-11-22 | 2018-04-13 | 昆山创匠新材料科技有限公司 | A kind of resin combination and preparation method thereof |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
| CN113278388A (en) * | 2021-04-26 | 2021-08-20 | 青岛歌尔微电子研究院有限公司 | Conductive silver adhesive and preparation method thereof |
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Application publication date: 20120509 |