CN103317148B - A kind of silver powder and gained elargol - Google Patents
A kind of silver powder and gained elargol Download PDFInfo
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- CN103317148B CN103317148B CN201310226590.5A CN201310226590A CN103317148B CN 103317148 B CN103317148 B CN 103317148B CN 201310226590 A CN201310226590 A CN 201310226590A CN 103317148 B CN103317148 B CN 103317148B
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- silver
- silver powder
- powder
- elargol
- epoxy resin
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Abstract
The present invention relates to chemical industry grout material field, be specifically related to a kind of silver powder and gained elargol.Silver powder it obtained by following processing step, A, high-temperature spray pyrolysis silver salt compound: the ethanolic solution pyrolytic reaction making silver salt on high-temperature spray pyrolysis plant, reaction terminates to form the spherical silver particle of 300-800nm; B, high speed ball milling: the silver powder particle of steps A gained is added in planetary ball mill, add the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking, high speed ball milling 5-8 hour, obtain narrowly distributing flake silver powder, the weight ratio of described silver powder particle and the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking is 1:(1.7-2.3): (4%-6%).The elargol product prepared with this silver powder has high-termal conductivity, high conductivity.<!--1-->
Description
Technical field
The present invention relates to chemical industry grout material field, be specifically related to a kind of silver powder and gained elargol.
Background technology
The optimum normal temperature electric conductivity of silver powder, optimum thermal conductivity and relative chemical stability, make it be widely used in modern industry, and along with the development of electronics industry, the electric conductivity of silver powder and thermal conductivity become the indispensable material of electronics industry.
Chinese patent application CN101279369 discloses a kind of preparation method of sheet silver powder with high dispersibility, it is characterized in that particle diameter D50 at 1 ~ 3 μm, the spherical raw material silver powder of silver content > 99.95%, grinder is adopted to grind to form flake silver powder, then improved by ultrasonic disperse, air dispersion post processing that it is dispersed, obtained sheet footpath D50 3 ~ 25 μm, apparent density is the flake silver powder of the polymolecularity of 0.5 ~ 1.8g/cm3.This preparation method's technological process is simple, is suitable for industrial large-scale production flake silver powder.Too low being not suitable for of the silver powder tap density that this patent discloses does high elargol of filling.Chinese patent application CN101214555 discloses a kind of method of spherical silver, add some copper nitrates, nickel nitrate or magnesium nitrate in the method to produce respective oxide when thermal decomposition and stop growing up of silver-colored crystal grain, acquisition particle diameter is 10-100nm, the product that narrowly distributing, sphericity are high, degree of crystallinity is high.
Summary of the invention
For above-mentioned technological deficiency, the technical issues that need to address of the present invention solve silver powder narrow diameter distribution, the problem that tap density is little.
For solving the problems of the technologies described above, technical scheme provided by the invention is: a kind of silver powder, and it is obtained by following processing step:
A, high-temperature spray pyrolysis silver salt compound: the ethanolic solution pyrolytic reaction making silver salt on high-temperature spray pyrolysis plant, reaction terminates the spherical silver particle forming 300-800nm;
B, high speed ball milling: the silver powder particle of steps A gained is added in planetary ball mill, add the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking, high speed ball milling 5-8 hour, obtain distribution flake silver powder, the weight ratio of described silver powder particle and the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking is 1:(1.7-2.3): (4%-6%).
Further: in above-mentioned silver powder, described silver compound refers at least one in silver nitrate, silver acetate or silver oxalate, and what preferably get is one or both in silver acetate or silver oxalate.D50=1-2 micron, D90=4 micron, namely D50 be meant to 50% silver powder particle diameter or diameter be less than 1-2 micron, D90 be meant to 90% be less than 4 microns, tap density reaches 4-5g/cm
3silver powder.
The present invention does not provide and obtains elargol with above-mentioned silver powder, it is obtained by following processing step, the mixture of silver powder and epoxy resin powder is solidified 1 ± 0.2 hour obtained elargol at 150 ± 10 DEG C, described silver powder and the percentage by weight of epoxy resin powder are (2.5-3): 1, and described curing agent accounts for 0.1% of silver powder and epoxy resin powder mixture weight.The described epoxy resin sphere of powder is bisphenol F epoxy resin, and described curing agent is imidazole curing agent.
Compared with prior art, silver powder of the present invention, it is obtained by following processing step, A, high-temperature spray pyrolysis silver salt compound: the ethanolic solution pyrolytic reaction making silver salt on high-temperature spray pyrolysis plant, and reaction terminates the spherical silver particle forming 300-800nm; B, high speed ball milling: the silver powder particle of steps A gained is added in planetary ball mill, add the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking, high speed ball milling 5-8 hour, obtain distribution flake silver powder, the weight ratio of described silver powder particle and the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking is 1:(1.7-2.3): (4%-6%).Obtain D50=1-2 micron, D90=4 micron, narrow distribution, tap density reaches 4-5g/cm
3silver powder, the elargol product prepared with this silver powder has high-termal conductivity, high conductivity.
Way of example
Purport of the present invention is by high-temperature spray pyrolysis silver salt compound and high speed ball milling silver powder, and obtain tap density high, the silver powder of narrow diameter distribution, the elargol product prepared with this silver powder has high-termal conductivity, high conductivity.Below in conjunction with embodiment, content of the present invention is described in further detail.
Embodiment 1
Be dissolved in the ethanol of 2L by 1000g silver acetate, spray pyrolysis temperature is 380 DEG C, obtains the ball shape silver powder that particle diameter is 500nm after pyrolysis.The weight ratio of described silver powder particle and the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking is 1:(1.7-2.3): (4%-6%)
100g ball shape silver powder is added in planetary ball mill, then adds the acrylonitrile-butadiene rubber of 200g absolute ethyl alcohol and 5g carboxy blocking.Start ball mill, with the rotating speed ball milling 6 hours of 200rpm.
Analyze with PSA laser particle size analyzer, the particle diameter of silver powder is D50=1-2 micron, D90=4 micron.Tap density reaches 4-5g/cm
3
Embodiment 2
Be dissolved in the ethanol of 2L by 800g silver oxalate, other is identical with embodiment one.Analyze with PSA laser particle size analyzer, the particle diameter of silver powder is D50=1-2 micron, D90=4 micron.Tap density reaches 4-5g/cm
3.
Embodiment 3
Be dissolved in the ethanol of 2L by 1200g silver acetate and silver oxalate, other is identical with embodiment one.Analyze with PSA laser particle size analyzer, the particle diameter of silver powder is D50=1-2 micron, D90=4 micron.Tap density reaches 4-5g/cm
3.
Embodiment 4
On the basis of embodiment 1-3,100g ball shape silver powder is added in planetary ball mill, then add the acrylonitrile-butadiene rubber of 180g absolute ethyl alcohol and 6g carboxy blocking.Analyze with PSA laser particle size analyzer, the particle diameter of silver powder is D50=1-2 micron, and D90=4 micron, tap density reaches 4-5g/cm
3.
Embodiment 5
On the basis of embodiment 1-3,100g ball shape silver powder is added in planetary ball mill, then add the acrylonitrile-butadiene rubber of 220g absolute ethyl alcohol and 4g carboxy blocking.Analyze with PSA laser particle size analyzer, the particle diameter of silver powder is D50=1-2 micron, D90=4 micron.Tap density reaches 4-5g/cm
3.
Application examples 1
Get respectively and the silver powder 73g of above-described embodiment 1-5 is joined in the bisphenol F epoxy resin of 27g, then add the imidazole curing agent of 0.1g, at 150 DEG C, solidify 60min, obtain electric conductivity and all good elargol of thermal conductivity.
After elargol of the present invention prepares, silk screen print method is adopted to print long L=10cm on common nonconducting glass plate, wide W=0.5cm, the batten of thickness h=10-100 μm, then curing reaction in an oven, tests the resistance R of gained batten with universal meter (U.S. FlukeF28II), calculate specific insulation ρ according to formula ρ=R*W*h/L, produce HC-110 thermal conductivity instrument with EKO company and test its thermal conductivity, elargol resistivity is less than 10
-4the Ω cm order of magnitude, most I reaches 10
-6the Ω cm order of magnitude.Thermal conductivity is not less than 2.5W/mK, maximumly reaches 10W/mK.
Application examples 2
Get respectively and the silver powder 81g of above-described embodiment 1-5 is joined in the bisphenol F epoxy resin of 27g, then add the imidazole curing agent of 0.1g, at 150 DEG C, solidify 60min, obtain electric conductivity and all good elargol of thermal conductivity.Elargol resistivity is less than 10
-4the Ω cm order of magnitude, most I reaches 10
-6the Ω cm order of magnitude.Thermal conductivity is not less than 2.5W/mK, maximumly reaches 10W/mK.
Above-described embodiment, just preferred embodiment of the present invention, is not used for limiting practical range of the present invention, therefore all equivalences done with the feature described in the claims in the present invention and principle change or modify, and all should be included within the claims in the present invention scope.
Claims (5)
1. a silver powder, is characterized in that: it is obtained by following processing step,
A, high-temperature spray pyrolysis silver salt compound: the ethanolic solution pyrolytic reaction making silver salt on high-temperature spray pyrolysis plant, reaction terminates the ball shape silver powder particle forming 300-800nm;
B, high speed ball milling: the ball shape silver powder particle of steps A gained is added in planetary ball mill, add the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking, high speed ball milling 5-8 hour, obtain flake silver powder, the weight ratio of described ball shape silver powder particle and the acrylonitrile-butadiene rubber of absolute ethyl alcohol and carboxy blocking is 1:(1.7-2.3): (4%-6%);
The silver powder particle diameter of 90% is less than 4 microns, and the tap density of silver powder reaches 4-5g/cm
3.
2. silver powder according to claim 1, is characterized in that: described silver salt compound refers at least one in silver nitrate, silver acetate or silver oxalate.
3. silver powder according to claim 2, is characterized in that: described silver salt compound is one or both in silver acetate or silver oxalate.
4. the elargol obtained with silver powder described in any one in claim 1-3, it is characterized in that: it is obtained by following processing step, the mixture of silver powder and epoxy resin powder is solidified obtained elargol in curing agent, solidification temperature is 150 ± 10 DEG C, hardening time is 1 ± 0.2 hour, described silver powder and the percentage by weight of epoxy resin powder are (2.5-3): 1, and described curing agent accounts for 0.1% of silver powder and epoxy resin powder mixture weight.
5. elargol according to claim 4, is characterized in that: described epoxy resin powder is bisphenol F epoxy resin, and described curing agent is imidazole curing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310226590.5A CN103317148B (en) | 2013-06-07 | 2013-06-07 | A kind of silver powder and gained elargol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310226590.5A CN103317148B (en) | 2013-06-07 | 2013-06-07 | A kind of silver powder and gained elargol |
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| CN103317148A CN103317148A (en) | 2013-09-25 |
| CN103317148B true CN103317148B (en) | 2015-11-25 |
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| CN105985745A (en) * | 2015-01-30 | 2016-10-05 | 上海蓝沛信泰光电科技有限公司 | Anisotropic conductive adhesive applied on EMI shielding film, and preparation method thereof |
| JP6404261B2 (en) * | 2016-05-17 | 2018-10-10 | トクセン工業株式会社 | Silver powder |
| CN111117537A (en) * | 2019-07-12 | 2020-05-08 | 杭州正银电子材料有限公司 | Efficient photovoltaic laminated tile conductive adhesive and preparation method thereof |
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| CN1548260A (en) * | 2003-05-12 | 2004-11-24 | 贵研铂业股份有限公司 | Surface processing method of superfine silver powder |
| CN1736636A (en) * | 2005-09-12 | 2006-02-22 | 昆明理工恒达科技有限公司 | Low loose density sheet-like silver powder preparation method |
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000265202A (en) * | 1999-03-12 | 2000-09-26 | Tanaka Kikinzoku Kogyo Kk | Production of silver powder |
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| CN1548260A (en) * | 2003-05-12 | 2004-11-24 | 贵研铂业股份有限公司 | Surface processing method of superfine silver powder |
| CN1736636A (en) * | 2005-09-12 | 2006-02-22 | 昆明理工恒达科技有限公司 | Low loose density sheet-like silver powder preparation method |
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
| CN102962473A (en) * | 2012-12-06 | 2013-03-13 | 云南铜业科技发展股份有限公司 | Method for preparing silver powder for touch screen silver paste |
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