CN105062398B - A kind of dual cure Frontal polymerization conductive silver glue and preparation method thereof - Google Patents
A kind of dual cure Frontal polymerization conductive silver glue and preparation method thereof Download PDFInfo
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- CN105062398B CN105062398B CN201510525048.9A CN201510525048A CN105062398B CN 105062398 B CN105062398 B CN 105062398B CN 201510525048 A CN201510525048 A CN 201510525048A CN 105062398 B CN105062398 B CN 105062398B
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Abstract
The present invention discloses a kind of dual cure Frontal polymerization conductive silver glue and preparation method thereof, can be with photocuring and heat cure, and using Frontal polymerization principle, conductive silver glue can reach deep cure.By epoxy resin, epoxy active diluent, light trigger, latency thermal initiator, antioxidant, ultra-violet absorber, coupling agent, dispersant and conducting particles are made by mixing, stirring, grinding distribution.The conducting resinl reaches deep layer thermal initiation by the light-initiated Frontal polymerization of utilization afterwards and is fully cured so as to reach, glue-line thickness solidification can be realized, there is good adherence after solidification, solvent resistance, resistivity is low, can meet LED chip, liquid crystal material, film resistor, the technology of the microelectronics Packaging such as pcb board needs.
Description
Technical field
The present invention relates to conducting resinl, and in particular to a kind of photocuring and heat cure reach that deep layer is consolidated using Frontal polymerization principle
The conductive silver glue of change.
Background technology
At present, conductive silver glue is that the conductive silver powder for providing electrical property is filled into the polymer sizing for providing mechanical performance
Obtained electronic chemical product, is that one kind can effectively bond various materials, and the adhesive of conductive energy.
Because conductive silver glue has a large amount of silver powder inserts, when glue-line is had certain thickness, light is being carried out by UV lamp
During solidification, the bottom of glue-line can not be absorbed to ultraviolet, and its main cause is that the resin in its raw material uses acrylate,
Light trigger decomposes the carbon-carbon double bond crosslinking curing produced in free radical initiation acrylate under UV lamp illumination, it is impossible to carry out thermosetting
Change, can only carry out photocuring by UV lamp, its reaction effect causes that the hardness of glue-line is low, cohesive force is small, glue-line is easily come off.
So in order to solve the problems, such as this respect, the present invention uses Frontal polymerization principle, when glue-line passes through UV lamp, pass through
Ultraviolet triggers the heat that upper strata adhesive curing is produced to trigger the heat cure of bottom glue so that reach deep cure without being filled out
Material blocks ultraviolet influence.
The content of the invention
Present invention aims at, overcome because conductive filler blocks ultraviolet light do not reach deep cure caused by cohesive force
Difference, can guarantee that the quality of product again while product efficiency is improved.
The object of the present invention is achieved like this：
A kind of dual cure Frontal polymerization conductive silver glue, it is characterized in that, it is composed of the following components in parts by mass：Asphalt mixtures modified by epoxy resin
15 ~ 25 parts of fat, 1 ~ 5 part of epoxide diluent, 2 ~ 3 parts of light trigger, 2 ~ 3 parts of latency thermal initiator, antioxidant 0.5 ~ 1
Part, 0.5 ~ 1 part of ultra-violet absorber, 0.5 ~ 1.5 part of coupling agent, 0..5 parts of dispersant, 70 ~ 80 parts of conductive silver powder；
The latency thermal initiator is thermal acid generator amine closing lewis acid.
In addition, the present invention also provides a kind of preparation method of dual cure Frontal polymerization conductive silver glue, it is characterized in that, including
Following steps,
（1）First weigh after epoxy resin add light trigger, thermal initiator, antioxidant, ultra-violet absorber, coupling agent,
Dispersed with stirring uniformly carries out three-roller and ground semi-finished product base-material to be made three times afterwards after dispersant；
（2）Weigh added after respective amount semi-finished product base-material corresponding conductive silver powder amount be stirred it is scattered after carry out three-roller and grind
Mill is scattered until below fineness 15um, obtains elargol；
（3）Elargol is added into deaeration machine and carries out deaeration 5 ~ 10 minutes, you can dual cure Frontal polymerization conductive silver glue is obtained.
The present invention can also be solved using following technical measures：
The epoxy resin is low-molecular-weight epoxy resin, specifically bisphenol A epoxide resin or bisphenol F epoxy resin or phenol
A kind of or multiple mixing of aldehyde epoxy or hydrogenated bisphenol A epoxy resin or resorcin epoxy resin or cycloaliphatic epoxy resin
Composition.
The viscosity of the low-molecular-weight epoxy resin is in 200 ~ 5000 mpa s.
The epoxide diluent is by the one of the unitary of alcohol or alicyclic ring alcohol or aromatic alcohol, binary or polynary glycidol ether
Plant or a variety of mixing compositions.
The light trigger is photoacid generator such as sulfosalt series, salt compounded of iodine series, sulfonic acid fat series, three nitrogen piperazines series,
The one or two kinds of mixing of specifically triaryl hexafluoro-antimonic acid sulfonium salt or hexafluorophosphoric acid salt compounded of iodine is constituted.
The latency thermal initiator is thermal acid generator amine closing lewis acid, specifically AgMSAF3- (fluoroform sulphurs
Acid) silver salt or SPh3SbF6- triaryl hexafluoro-antimonic acid sulfonium salts one or two kinds of mixing composition.
The antioxidant is that hindered phenol type kind antioxidant, specifically IRGANOX 1010 or IRGANOX 245 are constituted.
The ultra-violet absorber is benzophenone class or benzotriazole, specifically UV-P or UV-O；
The coupling agent is made up of DOW CORNING Z-6040, Z-6020, Z-6030 one or more kinds of mixing；
The dispersant is polyurethanes or esters of acrylic acid dispersant, and specifically enlightening high score powder or Bi Ke disperses
Agent is constituted.
Conductive silver powder is flake silver powder, and its particle diameter is at 0.5 ~ 10 micron, and tap density is in 2 ~ 4g/cm3.
The present invention uses Frontal polymerization reaction, and Frontal polymerization is a kind of hot for motive force with autoreactivity, by anti-
The continuous moving in region is answered, the polymerisation pattern of bulk polymerization conversion is finally realized.The present invention Frontal polymerization principle be exactly
It is motive force using photocuring reaction heat so that conversion zone（That is glue-line）Moved from top is continuous toward bottom, finally
Realize the reaction pattern of glue-line bulk polymerization conversion.
Its course of reaction is specifically：When glue-line passes through UV lamp, the light trigger of top glue-line is released under UV lamp illumination effect
Bronsted acid carry out ring-opening polymerization rapid to epoxy resin is put, reaction produces substantial amounts of heat, when heat transfer to bottom glue-line
When heat along with UV lamp in itself, excite latency thermal initiator, latency thermal initiator discharges proton under heat effect
Acid carry out ring-opening polymerization rapid to epoxy resin so that bottom glue-line carries out heat cure, allows whole glue-line to reach depth
Layer solidification.
The beneficial effects of the invention are as follows：
（1）, using Frontal polymerization principle, realize the perfect adaptation of photocuring and heat cure, be a kind of novel conductive elargol；
It had both improved production efficiency and has saved the energy, can guarantee that properties of product are not affected again.Overcome heat cure conductive silver
Adhesive curing speed is slow, while the shortcomings of cohesive force is poor caused by deep cure can not be reached by also overcoming light curable conductive elargol,
It is a kind of conductive silver glue of brand-new and excellent performance.
（2）, hardening time it is short, efficiency high, efficiency is traditional 2-3 times.
（3）, conductive and thermal conductivity it is good, specific insulation can reach 2 × 10-4 Ω .cm, and thermal conductivity factor is up to 10w/mk.
（4）, adhesive force it is good, hardness is up to 7H.
（5）The light trigger and latency thermal initiator of the present invention is cationic initiator, can be referred to as acid agent,
Bronsted acid can be produced, epoxy resin can carry out ring-opening polymerisation rapidly under Bronsted acid effect, so as to reach dual cure, effectively
The hardness for making glue-line, increase cohesive force are improved, makes glue-line difficult for drop-off, Adhesion enhancement.
Embodiment
With reference to embodiment, the present invention is further described.
1st embodiment：
（1）It is prepared by semi-finished product base-material：
3.5 parts of bisphenol A epoxide resin
Cycloaliphatic epoxy resin 15
2 parts of light trigger
2 parts of thermal initiator
Antioxidant 0.5
Ultra-violet absorber 0.5
1 part of coupling agent
Dispersant 0.5
It is that can obtain semi-finished product base-material that above-mentioned material dispersed with stirring is uniformly carried out to three-roller afterwards and grinds three times；
（2）It is prepared by conductive silver glue：
25 parts of semi-finished product base-material
75 parts of flake silver powder
Above-mentioned material dispersed with stirring is uniformly carried out to three-roller grinding afterwards until fineness 15um is following with elargol deaeration machine
Evacuation and centrifugal degassing can obtain dual cure Frontal polymerization conductive silver glue in 5 ~ 10 minutes.
2nd embodiment：
（1）It is prepared by semi-finished product base-material：
9 parts of hydrogenated bisphenol A epoxy resin
9.5 parts of cycloaliphatic epoxy resin
2 parts of light trigger
2 parts of thermal initiator
0.5 part of antioxidant
0.5 part of ultra-violet absorber
1 part of coupling agent
0.5 part of dispersant
It is that can obtain semi-finished product base-material that above-mentioned material dispersed with stirring is uniformly carried out to three-roller afterwards and grinds three times；
（2）It is prepared by conductive silver glue：
25 parts of semi-finished product base-material
75 parts of flake silver powder
Above-mentioned material dispersed with stirring is uniformly carried out to three-roller grinding afterwards until fineness 15um is following with elargol deaeration machine
Evacuation and centrifugal degassing can obtain dual cure Frontal polymerization conductive silver glue in 5 ~ 10 minutes.
The present embodiment, which adds hydrogenated bisphenol A, can be made the conductive silver glue of more high conductivity.
3rd embodiment：
（1）It is prepared by semi-finished product base-material：
5 parts of novolac epoxy resin
18.5 parts of cycloaliphatic epoxy resin
2 parts of light trigger
2 parts of thermal initiator
Antioxidant 0.5
Ultra-violet absorber 0.5
1 part of coupling agent
Dispersant 0.5
It is that can obtain semi-finished product base-material that above-mentioned material dispersed with stirring is uniformly carried out to three-roller afterwards and grinds three times；
（2）It is prepared by conductive silver glue：
30 parts of semi-finished product base-material
70 parts of flake silver powder
Above-mentioned material dispersed with stirring is uniformly carried out to three-roller grinding afterwards until fineness 15um is following with elargol deaeration machine
Evacuation and centrifugal degassing can obtain dual cure Frontal polymerization conductive silver glue in 5 ~ 10 minutes.
It is to improve hardness and heat resistance after monolithic conductive adhesive curing that the present embodiment, which adds novolac epoxy resin,.
The present invention is triggered the heat cure of underfill resin layer by UV photocurings, is possessed following beneficial effect by conductive silver glue：
1st, hardening time is short, efficiency high, and efficiency is traditional 2-3 times.
2nd, conductive and thermal conductivity is good, and specific insulation can reach 2 × 10-4 Ω .cm, and thermal conductivity factor is up to 10w/mk.
3rd, adhesive force is good, and hardness is up to 7H.
The present invention uses Frontal polymerization reaction, and Frontal polymerization is a kind of hot for motive force with autoreactivity, by anti-
The continuous moving in region is answered, the polymerisation pattern of bulk polymerization conversion is finally realized.The present invention Frontal polymerization principle be exactly
It is motive force using photocuring reaction heat so that conversion zone（That is glue-line）Moved from top is continuous toward bottom, finally
Realize the reaction pattern of glue-line bulk polymerization conversion.
Its course of reaction is specifically：When the glue-line prepared by above-described embodiment passes through UV lamp, top glue-line it is light-initiated
Agent discharges Bronsted acid carry out ring-opening polymerization rapid to epoxy resin under UV lamp illumination effect, and reaction produces substantial amounts of heat,
Heat when heat transfer is to bottom glue-line along with UV lamp in itself, excites latency thermal initiator, latency thermal initiator
Bronsted acid carry out ring-opening polymerization rapid to epoxy resin is discharged under heat effect so that bottom glue-line carries out heat cure,
Whole glue-line is set to reach deep cure.
Particular embodiments described above, only preferred embodiments of the present invention, such as according to the present patent application patent
The equivalent arrangements that scope is done, the technology that should be the present invention is covered.
Claims (6)
1. a kind of preparation method of dual cure Frontal polymerization conductive silver glue, it is characterized in that, in parts by mass by following components group
Into：15 ~ 25 parts of epoxy resin, 1 ~ 5 part of epoxide diluent, 2 ~ 3 parts of light trigger, 2 ~ 3 parts of latency thermal initiator, antioxidant
0.5 ~ 1 part, 0.5 ~ 1 part of ultra-violet absorber, 0.5 ~ 1.5 part of coupling agent, 0.5 part of dispersant, 70 ~ 80 parts of conductive silver powder；
The latency thermal initiator is thermal acid generator amine closing lewis acid；
The epoxy resin is low-molecular-weight epoxy resin, specifically bisphenol A epoxide resin or bisphenol F epoxy resin or phenolic aldehyde ring
A kind of or multiple mixing group of oxygen or hydrogenated bisphenol A epoxy resin or resorcin epoxy resin or cycloaliphatic epoxy resin
Into；
The viscosity of the low-molecular-weight epoxy resin is in 200 ~ 5000 mpas；
Conductive silver powder is flake silver powder, and its particle diameter is at 0.5 ~ 10 micron, and tap density is in 2 ~ 4g/cm3；
Its preparation method, comprises the following steps；
（1）First weigh and light trigger added after epoxy resin, it is thermal initiator, antioxidant, ultra-violet absorber, coupling agent, scattered
Dispersed with stirring uniformly carries out three-roller and ground semi-finished product base-material to be made three times afterwards after agent；
（2）Weigh added after respective amount semi-finished product base-material corresponding conductive silver powder amount be stirred it is scattered after carry out three-roller grinding point
Dissipate until below fineness 15um, obtain elargol；
（3）Elargol is added into deaeration machine and carries out deaeration 5 ~ 10 minutes, you can dual cure Frontal polymerization conductive silver glue is obtained；
When elargol passes through UV lamp, the light trigger of the top glue-line release Bronsted acid under UV lamp illumination effect is rapid to epoxy resin
Ring-opening polymerization is carried out, reacts and produces substantial amounts of heat, the heat when heat transfer is to bottom glue-line along with UV lamp in itself,
Latency thermal initiator is excited, latency thermal initiator discharges Bronsted acid carry out open loop rapid to epoxy resin under heat effect
Polymerisation so that bottom glue-line carries out heat cure, allows whole elargol to reach deep cure.
2. the preparation method of dual cure Frontal polymerization conductive silver glue according to claim 1, it is characterised in that the epoxy
Diluent is one or more kinds of mixing groups by the unitary of alcohol or alicyclic ring alcohol or aromatic alcohol, binary or polynary glycidol ether
Into.
3. the preparation method of dual cure Frontal polymerization conductive silver glue according to claim 1, it is characterised in that the light draws
It is photoacid generator to send out agent, specifically the one or two kinds of mixing group of triaryl hexafluoro-antimonic acid sulfonium salt or hexafluorophosphoric acid salt compounded of iodine
Into.
4. the preparation method of dual cure Frontal polymerization conductive silver glue according to claim 1, it is characterised in that described latent
Property thermal initiator be thermal acid generator amine closing lewis acid, specifically AgMSAF3- (trifluoromethanesulfonic acid) silver salt or
The one or two kinds of mixing composition of SPh3SbF6- triaryl hexafluoro-antimonic acid sulfonium salts.
5. the preparation method of dual cure Frontal polymerization conductive silver glue according to claim 1, it is characterised in that the antioxygen
Agent is that hindered phenol type kind antioxidant, specifically IRGANOX 1010 or IRGANOX 245 are constituted.
6. the preparation method of dual cure Frontal polymerization conductive silver glue according to claim 1, it is characterised in that described ultraviolet
Light absorbers are benzophenone class or benzotriazole, specifically UV-P or UV-O；
The coupling agent is made up of DOW CORNING Z-6040, Z-6020, Z-6030 one or more kinds of mixing；
The dispersant is polyurethanes or esters of acrylic acid dispersant, specifically enlightening high score powder or Bi Ke dispersant groups
Into.
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| CN105405489A (en) * | 2015-12-16 | 2016-03-16 | 佛山市顺德区百锐新电子材料有限公司 | Low-temperature cured and weldable high-conductivity slurry and preparation method thereof |
| TWI595073B (en) * | 2016-01-28 | 2017-08-11 | 光洋應用材料科技股份有限公司 | Conductive Silver Adhesive And Conductive Silver Layer |
| CN106085276B (en) * | 2016-07-07 | 2019-03-29 | 深圳先进技术研究院 | A kind of conductive silver glue and the preparation method and application thereof adulterating silver salt |
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| CN106675501A (en) * | 2017-01-09 | 2017-05-17 | 成都科愿慧希科技有限公司 | Dual-cured electrically-conductive silver adhesive |
| CN106753139A (en) * | 2017-01-20 | 2017-05-31 | 杭州宝明新材料科技有限公司 | A kind of one-component epoxy resin adhesive of retardation of curing |
| CN107446520B (en) * | 2017-06-29 | 2019-03-01 | 晶丰电子封装材料（武汉）有限公司 | A kind of normal temperature cure conducting resinl and its process for connecting rechargeable battery pack |
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| CN108130029A (en) * | 2017-12-22 | 2018-06-08 | 烟台德邦科技有限公司 | A kind of conductive silver glue of UV retardation of curing and preparation method thereof |
| CN108659463B (en) * | 2018-04-24 | 2020-06-02 | 珠海元盛电子科技股份有限公司 | Photocuring high-thermal-conductivity and electric-conductivity hole plugging material for printed circuit board and preparation method thereof |
| CN109852143B (en) * | 2019-02-26 | 2021-08-24 | 江门市阪桥电子材料有限公司 | UV-LED ink-jet printing black character ink and preparation method thereof |
| CN112054322A (en) * | 2020-09-04 | 2020-12-08 | 立讯精密工业股份有限公司 | Connecting structure of cable and PCB, plug assembly adopting connecting structure and preparation method of plug assembly |
| CN116376492A (en) * | 2023-05-19 | 2023-07-04 | 思特迪新材料科技(深圳)有限公司 | Dual-cured conductive silver adhesive and preparation method thereof |
| CN117165236B (en) * | 2023-10-30 | 2024-04-12 | 空净视界智能科技有限公司 | Insulating die bond adhesive for LED and preparation method thereof |
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| CN101747855B (en) * | 2010-01-18 | 2013-08-14 | 北京海斯迪克新材料有限公司 | Low-resistivity single-component conductive silver paste and preparation method thereof |
| CN102127386B (en) * | 2010-12-29 | 2013-11-20 | 东莞市新懿电子材料技术有限公司 | Photocuring and thermocuring conductive adhesive and preparation method |
| CN102504745B (en) * | 2011-11-09 | 2013-09-04 | 烟台德邦科技有限公司 | Double curing encapsulating adhesive and preparation method thereof |
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Effective date of registration: 20211129 Address after: 528000 No. 31, South Road, Lunjiao Yongfeng Village Committee Industrial Zone, Shunde District, Foshan City, Guangdong Province Patentee after: FOSHAN SHUNDE BAIRUI NEW ELECTRONIC MATERIALS Co.,Ltd. Patentee after: Tongbai Hongxin New Material Co., Ltd Address before: 528308 No. 31, South Road, Yongfeng Village Committee Industrial Zone, Lunjiao sub district office, Shunde District, Foshan City, Guangdong Province Patentee before: FOSHAN SHUNDE BAIRUI NEW ELECTRONIC MATERIALS Co.,Ltd. |
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