CN105405489A - Low-temperature cured and weldable high-conductivity slurry and preparation method thereof - Google Patents
Low-temperature cured and weldable high-conductivity slurry and preparation method thereof Download PDFInfo
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- CN105405489A CN105405489A CN201510938971.5A CN201510938971A CN105405489A CN 105405489 A CN105405489 A CN 105405489A CN 201510938971 A CN201510938971 A CN 201510938971A CN 105405489 A CN105405489 A CN 105405489A
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
The invention discloses a low-temperature cured and weldable high-conductivity slurry and a preparation method thereof. The low-temperature cured and weldable high-conductivity slurry is extremely strong in printing adaptability, contains a single component, can be cured rapidly at a low temperature, has an extremely good adhesive force, strong welding fastness and ultralow electrical resistivity, is suitable for 100-200 meshes silk-screen printing and dispensing and is mainly used in the fields of electronic circuits such as welding of PET, glass, ceramic, metal, circuit boards and solar silicon boards. The low-temperature cured and weldable high-conductivity slurry is prepared by mixing, stirring, grinding and dispersing high temperature resistant epoxy resin, a diluent, a latent thermal curing agent, a stabilizer, an antioxidant, a coupling agent, a dispersant and conducting particles.
Description
Technical field
The present invention relates to a kind of electrocondution slurry, be specifically related to welding high-conductivity slurry of a kind of low-temperature setting and preparation method thereof, belong to electric conducting material field.
Background technology
At present, can soldering paste be high-temperature sintered silver paste, but high-temperature sintered silver paste needs film forming after temperature 800 DEG C sinters, and has very high requirement to the temperature tolerance of ground, and energy consumption is large, equipment investment be high.After common silver slurry printing film forming not proper alignment time about 240 DEG C welding temperatures cause silver slurry adhesive force to decline, cause silver slurry to come off, make to weld.Someone obtains slurry by trial high-temperature resistant silicone, but organosilicon poor adhesive force, and the problems such as hardness is low, do not obtain very effectively achievement.
Summary of the invention
For solving the problem, the present invention utilizes high-temperature-resistant epoxy resin, can make in 140 ~ 150 DEG C of bakings, 5 ~ 10 minutes obtained hardness high, strong adhesion, TG point is at 300 ~ 400 DEG C, good conductivity and can proper alignment temperature slurry, is suitable for the electronic circuit field such as PET, glass, pottery, metal, wiring board, the welding of solar power silicon plate.
The object of the present invention is achieved like this:
The welding high-conductivity slurry of a kind of low-temperature setting, is characterized in that, composed of the following components by mass parts: resin semi-finished product 15-30 part, diluent 1-10 part, antioxidant 0.5-1 part, coupling agent 0.5-1.5 part, dispersant 0.5 part, conductive powder 70-85 part;
Described resin semi-finished product are composed of the following components by mass parts: high-temperature-resistant epoxy resin 10-25 part, latency thermal initiator 0.2-0.5 part, stabilizer 0.05-0.2 part.
The present invention can also adopt following technical measures to solve:
High-temperature-resistant epoxy resin adopts but is not limited to wherein one or both mixing compositions of low degree of functionality cycloaliphatic epoxy resin and polyfunctionality cycloaliphatic epoxy resin, alicyclic ring skeleton directly there is inner epoxy radicals, so there is excellent characteristic in curability and solidfied material physical property, TG point can be reached after its resin solidification and be greater than 300 DEG C, can be mixed by one or more.
Diluent is high boiling solvent; As nylon acid methyl esters (DBE), one or more the mixing of the high boiling solvents such as diethylene glycol monoethyl ether acetic acid esters (CA).
Latency thermal curing agents is the lewis acid that amine is closed; Specifically AgMSAF
3-(trifluoromethanesulfonic acid) silver salt or SPh
3sbF
6the one of-triaryl hexafluoro-antimonic acid sulfonium salt or two kinds of mixing compositions; Curing mechanism of the present invention be amine close lewis acid along with temperature raise reach initiation temperature after, release Bronsted acid carries out ring-opening polymerization rapidly to epoxy resin, rapid curing can be reached, thus save time and energy, reach high efficiency, carried out amine due to its activity to close, so can obtain one-component slurry, 25 DEG C of normal temperature can be placed for 3 ~ June and not affect size performance.
Stabilizer is nitrogenous epoxy resin stabilizer; By hindering proton transfer thus allowing stable system.
Antioxidant is hindered phenol type kind antioxidant; Specifically IRGANOX1010 or IRGANOX245 is wherein a kind of.
Coupling agent is silane coupler; Can be made up of one or more mixing of DOW CORNING Z-6040, Z-6020, Z-6030.
Dispersant is polyurethanes or esters of acrylic acid dispersant; Specifically enlightening high score powder or Bi Ke dispersant wherein a kind of.
Conductive silver powder is that flake silver powder or flake copper or Nickel Powder are wherein a kind of, and its particle size range is at 0.5 ~ 10 micron, and tap density is at 2 ~ 5.5g/cm
3.
Object of the present invention also comprises a kind of preparation method preparing the welding high-conductivity slurry of low-temperature setting, and it is characterized in that, its preparation method comprises the steps:
(1) add latency thermal curing agents, stabilizer after first taking high-temperature-resistant epoxy resin, dissolve obtained resin semi-finished product by constant temperature 40 DEG C of high speed dispersion;
(2) add after taking respective amount resin semi-finished product after corresponding diluent, coupling agent, antioxidant, dispersant and conductive powder carry out dispersed with stirring and carry out three-roller grinding distribution until below fineness 15um, obtain slurry.
The invention has the beneficial effects as follows:
(1) slurry of the present invention can 140 ~ 150 DEG C of low-temperature settings can soldering paste, do not need high temperature sintering, can be used for the ground of non-refractory.
(2) the present invention adopts high temperature resistant low degree of functionality cycloaliphatic epoxy resin and high temperature resistant polyfunctionality cycloaliphatic epoxy resin to be all the TG point epoxy resin that is greater than 300 DEG C after solidification, can proper alignment temperature (about 240 DEG C), and obtained slurry is different from common silver and starches.
(3) in slurry of the present invention, after resin solidification, adhesive force is good and hardness is high, is different from silicone based silver slurry.
(4) latency thermal curing agents of the present invention (about 100 DEG C) release Bronsted acid after reaching initiation temperature, to the rapid ring-opening polymerisation of epoxy resin, thus reach rapid curing, about 5 ~ 10 minutes curing times, energy efficient and time, enhance productivity to reach.
(5) resin of the present invention adopts the collocation of high temperature resistant low degree of functionality cycloaliphatic epoxy resin (low viscosity) and high temperature resistant polyfunctionality cycloaliphatic epoxy resin (high viscosity or solid) use can obtain good fluidity has body bone and the adaptable slurry of printing, can obtain electrically high after solidification.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
First embodiment, the preparation of silver slurry:
(1) the half-finished preparation of resin:
High temperature resistant low degree of functionality cycloaliphatic epoxy resin: 10 parts (about 350 DEG C of epoxide equivalent about 100 ~ 130, TG point);
High temperature resistant polyfunctionality cycloaliphatic epoxy resin: 10 parts (about 320 DEG C of epoxide equivalent about 150 ~ 200, TG point);
Latency thermal curing agents: 0.4 part;
Stabilizer: 0.2 part;
Resin semi-finished product are obtained by the above-mentioned component constant temperature taken 40 DEG C of high speed dispersion being dissolved;
High temperature resistant low degree of functionality cycloaliphatic epoxy resin, viscosity is approximately 25 DEG C of 100 ~ 240mPas, wetability is poor, and high temperature resistant polyfunctionality cycloaliphatic epoxy resin is high viscosity or hard resin, wetability is good, and collocation use can obtain good fluidity, and body bone is good, the slurry that printing adaptability is strong, can obtain high conductivity after hardening;
(2) slurry preparation:
Resin semi-finished product: 20.6 powder;
Diluent: 5 parts;
Antioxidant: 0.5 part;
Coupling agent: 1 part;
Dispersant: 0.5 part;
Silver powder: 72.4 parts;
After the above-mentioned component taken is carried out dispersed with stirring, carry out three-roller grinding distribution until below fineness 15um, obtain silver slurry.
Silver slurry was used 200 mesh web plates to be printed on to carry out 150 DEG C of bakings after on ground and within 10 minutes, welding film can be obtained, and recorded specific insulation and be approximately 0.8 ~ 1.5 × 10
-4Ω cm, adhesive force is 5B, and hardness can reach 5H ~ 7H.
Second embodiment, the preparation of copper slurry:
(1) the half-finished preparation of resin:
High temperature resistant low degree of functionality cycloaliphatic epoxy resin: 10 parts (about 350 DEG C of epoxide equivalent about 100 ~ 130, TG point);
High temperature resistant polyfunctionality cycloaliphatic epoxy resin: 10 parts (about 320 DEG C of epoxide equivalent about 150 ~ 200, TG point);
Latency thermal curing agents: 0.4 part;
Stabilizer: 0.2 part;
Resin semi-finished product are obtained by the above-mentioned component constant temperature taken 40 DEG C of high speed dispersion being dissolved;
(2) slurry preparation:
Resin semi-finished product: 20.6 powder;
Diluent: 5 parts;
Antioxidant: 0.5 part;
Coupling agent: 1 part;
Dispersant: 0.5 part;
Copper powder: 72.4 parts;
After the above-mentioned component taken is carried out dispersed with stirring, carry out three-roller grinding distribution until below fineness 15um, obtain copper slurry.
Copper slurry was used 200 mesh web plates to be printed on to carry out 150 DEG C of bakings after on ground and within 10 minutes, welding film can be obtained, and recorded specific insulation and be approximately 4 ~ 5 × 10
-4Ω cm, adhesive force is 5B, and hardness can reach 5H ~ 7H.
Above-described specific embodiment, is only preferred embodiment of the present invention, such as according to the equivalent arrangements that the present patent application the scope of the claims does, all should be technology of the present invention and contained.
Claims (10)
1. the welding high-conductivity slurry of low-temperature setting, is characterized in that, composed of the following components by mass parts: resin semi-finished product 15-30 part, diluent 1-10 part, antioxidant 0.5-1 part, coupling agent 0.5-1.5 part, dispersant 0.5 part, conductive powder 70-85 part;
Described resin semi-finished product are composed of the following components by mass parts: high-temperature-resistant epoxy resin 10-25 part, latency thermal initiator 0.2-0.5 part, stabilizer 0.05-0.2 part.
2. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, high-temperature-resistant epoxy resin adopts wherein one or both mixing compositions of low degree of functionality cycloaliphatic epoxy resin and polyfunctionality cycloaliphatic epoxy resin, can reach TG point and be greater than 300 DEG C after its resin solidification.
3. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, diluent is high boiling solvent.
4. the welding high-conductivity slurry of low-temperature setting according to claim 1, is characterized in that, latency thermal curing agents is the lewis acid that amine is closed.
5. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, stabilizer is nitrogenous epoxy resin stabilizer.
6. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, antioxidant is hindered phenol type kind antioxidant.
7. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, coupling agent is silane coupler.
8. the welding high-conductivity slurry of low-temperature setting according to claim 1, it is characterized in that, dispersant is polyurethanes or esters of acrylic acid dispersant.
9. the welding high-conductivity slurry of low-temperature setting according to claim 1, is characterized in that, conductive silver powder is that flake silver powder or flake copper or Nickel Powder are wherein a kind of, and its particle size range is at 0.5 ~ 10 micron, and tap density is at 2 ~ 5.5g/cm
3.
10. prepare a preparation method for the welding high-conductivity slurry of low-temperature setting, it is characterized in that, its preparation method comprises the steps:
(1) add latency thermal curing agents, stabilizer after first taking high-temperature-resistant epoxy resin, dissolve obtained resin semi-finished product by constant temperature 40 DEG C of high speed dispersion;
(2) add after taking respective amount resin semi-finished product after corresponding diluent, coupling agent, antioxidant, dispersant and conductive powder carry out dispersed with stirring and carry out three-roller grinding distribution until below fineness 15um, obtain slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510938971.5A CN105405489A (en) | 2015-12-16 | 2015-12-16 | Low-temperature cured and weldable high-conductivity slurry and preparation method thereof |
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|---|---|---|---|
| CN201510938971.5A CN105405489A (en) | 2015-12-16 | 2015-12-16 | Low-temperature cured and weldable high-conductivity slurry and preparation method thereof |
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| CN105405489A true CN105405489A (en) | 2016-03-16 |
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| CN201510938971.5A Pending CN105405489A (en) | 2015-12-16 | 2015-12-16 | Low-temperature cured and weldable high-conductivity slurry and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108130036A (en) * | 2017-12-18 | 2018-06-08 | 深圳市思迈科新材料有限公司 | Flexible splicing conducting resinl and preparation method thereof |
| CN109065217A (en) * | 2018-08-10 | 2018-12-21 | 深圳市思迈科新材料有限公司 | HJT solar low-temperature conductive silver paste and the preparation method and application thereof |
| CN109648221A (en) * | 2018-11-29 | 2019-04-19 | 中国科学院电工研究所 | A kind of soldering electric slurry and its preparation method and application |
| CN110875099A (en) * | 2018-08-31 | 2020-03-10 | 苏州晶银新材料股份有限公司 | Low-temperature conductive silver paste, preparation method thereof and product containing low-temperature conductive silver paste |
| CN114709005A (en) * | 2022-03-29 | 2022-07-05 | 深圳市百柔新材料技术有限公司 | Silver paste for flexible transparent conductive film metal grid, preparation method and application thereof |
| CN117165236A (en) * | 2023-10-30 | 2023-12-05 | 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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| JP2004264031A (en) * | 2003-01-23 | 2004-09-24 | Matsushita Electric Ind Co Ltd | Method for measuring conductive particle |
| CN102634290A (en) * | 2012-04-16 | 2012-08-15 | 江苏泰特尔化工有限公司 | Double-component transparent epoxy resin LED (light emitting diode) patch packing adhesive |
| CN102719213A (en) * | 2012-07-06 | 2012-10-10 | 江苏泰特尔化工有限公司 | Modified nano zinc oxide doped cycloaliphatic epoxy resin light-emitting diode (LED) packaging adhesive |
| CN103146259A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Screen printing conductive printing ink composition and preparation method thereof |
| CN105062398A (en) * | 2015-08-25 | 2015-11-18 | 佛山市顺德区百锐新电子材料有限公司 | Double-curing frontal polymerization conductive silver adhesive and preparing method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004264031A (en) * | 2003-01-23 | 2004-09-24 | Matsushita Electric Ind Co Ltd | Method for measuring conductive particle |
| CN102634290A (en) * | 2012-04-16 | 2012-08-15 | 江苏泰特尔化工有限公司 | Double-component transparent epoxy resin LED (light emitting diode) patch packing adhesive |
| CN102719213A (en) * | 2012-07-06 | 2012-10-10 | 江苏泰特尔化工有限公司 | Modified nano zinc oxide doped cycloaliphatic epoxy resin light-emitting diode (LED) packaging adhesive |
| CN103146259A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Screen printing conductive printing ink composition and preparation method thereof |
| CN105062398A (en) * | 2015-08-25 | 2015-11-18 | 佛山市顺德区百锐新电子材料有限公司 | Double-curing frontal polymerization conductive silver adhesive and preparing method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108130036A (en) * | 2017-12-18 | 2018-06-08 | 深圳市思迈科新材料有限公司 | Flexible splicing conducting resinl and preparation method thereof |
| CN109065217A (en) * | 2018-08-10 | 2018-12-21 | 深圳市思迈科新材料有限公司 | HJT solar low-temperature conductive silver paste and the preparation method and application thereof |
| CN110875099A (en) * | 2018-08-31 | 2020-03-10 | 苏州晶银新材料股份有限公司 | Low-temperature conductive silver paste, preparation method thereof and product containing low-temperature conductive silver paste |
| CN110875099B (en) * | 2018-08-31 | 2021-07-30 | 苏州晶银新材料股份有限公司 | Low-temperature conductive silver paste, preparation method thereof and product containing low-temperature conductive silver paste |
| CN109648221A (en) * | 2018-11-29 | 2019-04-19 | 中国科学院电工研究所 | A kind of soldering electric slurry and its preparation method and application |
| CN114709005A (en) * | 2022-03-29 | 2022-07-05 | 深圳市百柔新材料技术有限公司 | Silver paste for flexible transparent conductive film metal grid, preparation method and application thereof |
| CN117165236A (en) * | 2023-10-30 | 2023-12-05 | 空净视界智能科技有限公司 | Insulating die bond adhesive for LED 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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Application publication date: 20160316 |