CN104505151B - Chromium-containing high-dispersity conductive silver paste - Google Patents
Chromium-containing high-dispersity conductive silver paste Download PDFInfo
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- CN104505151B CN104505151B CN201410775520.XA CN201410775520A CN104505151B CN 104505151 B CN104505151 B CN 104505151B CN 201410775520 A CN201410775520 A CN 201410775520A CN 104505151 B CN104505151 B CN 104505151B
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Abstract
The invention discloses chromium-containing high-dispersity conductive silver paste. The chromium-containing high-dispersity conductive silver paste is prepared from the following raw materials in parts by weight: 100-107 parts of high-dispersity conductive silver powder, 0.4-0.6 part of glycerol monostearate, 25-30 parts of diethylene glycol ether acetate, 4-6 parts of butanone, 14-20 parts of polyamide, 0.5-1 part of N-methyl pyrrolidinone, 1-1.3 parts of 2-butoxy ethanol, 1-2 parts of trioctyl trimellitate, 0.1-0.2 part of chromium methionine, 1-2 parts of diammonium phosphate, 10-15 parts of glass powder and 0.6-1 part of calcium acetylacetone. According to the chromium-containing high-dispersity conductive silver paste, the high-dispersity conductive silver powder is nano silver powder and coats the surfaces of macromolecular microspheres in a uniform and dense manner, so that the consumption of precious-metal silver powder can be lowered, the production cost is reduced, and meanwhile, the dispersity and stability of the nano silver powder are greatly improved.
Description
Technical field
The invention mainly relates to conductive silver paste field, more particularly to a kind of high dispersive conductive silver paste containing chromium.
Background technology
Metallic silver particles are adopted in traditional conductive silver paste as the main component of silver paste, its electric conductivity is also to come real by it
Existing, it is uniformly distributed in bonding agent, before printing, makes serosity constitute the print material of certain viscosity, after printing, makes silver paste
Form stable combination between microgranule and base material, but due to silver metal price it is relatively expensive, it is possible to be considered as silver-colored cladding
Mode reducing the cost of metallic silver particles.
The content of the invention
The object of the invention is just to provide a kind of high dispersive conductive silver paste containing chromium.
The present invention is achieved by the following technical solutions：
A kind of high dispersive conductive silver paste containing chromium, it is characterised in that it is made up of the raw material of following weight parts：
High dispersive conductive silver powder 100-107, stearic acid monoglyceride 0.4-0.6, diethylene glycol ether acetate 25-30,
Butanone 4-6, polyamide 14-20, N-Methyl pyrrolidone 0.5-1, butoxy ethanol 1-1.3, trioctyl trimellitate (TOTM) 1-2,
Chromium methionine 0.1-0.2, Diammonium phosphate (DAP) 1-2, glass dust 10-15, calcium acetylacetonate 0.6-1；
What described high dispersive conductive silver powder was made up of the raw material of following weight parts：
Nano aluminium oxide 5-10, di-n-octyl sebacate 0.1-0.2, deionized water 300-400, styrene 4-7, alkyl phenol gather
Oxygen vinyl Ether 0.8-1, silane coupler KH560 1-2, Ammonium persulfate. 0.01-0.02, silver nitrate 131-140, polyvinyl pyrrole
Alkanone 1-2, sodium hypophosphite 30-40, three (nonyl phenyl) phosphite 2-3；
By nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 mixing, 500-700 rev/min of stirring mixing 20-
30 minutes, addition styrene, alkylphenol polyoxyethylene, the 30-35% of deionized water weight, magnetic agitation 40-50 minute, plus
Enter Ammonium persulfate., ultrasonic wave concussion 10-15h obtains nanoemulsions；
Silver nitrate, polyvinylpyrrolidone are mixed, the 40-50% of remaining deionized water weight is added, are stirred,
Obtain oxidation solution；
Remaining each raw material is mixed, Deca ammonia, regulation PH is 10-10.5, is reducing solution；
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions are added after completion of dropping, stirring reaction 30-50 minute,
Centrifugation, deionized water and washing with alcohol 3-5 time, drying, obtain final product.
A kind of preparation method of the high dispersive conductive silver paste containing chromium as claimed in claim 1, it is characterised in that include with
Lower step：
（1）Chromium methionine is added in butoxy ethanol, at being stirring evenly and then adding into calcium acetylacetonate, 60-70 DEG C
Stirring mixing 6-10 minutes, obtain dispersant；
（2）Polyamide is added in diethylene glycol ether acetate, trioctyl trimellitate (TOTM), fourth is stirring evenly and then adding into
Ketone, the stirring mixing 4-5 minutes at 70-80 DEG C, adds dispersant, 60-100 rev/min of dispersed with stirring 3-5 minute, must have airborne
Body；
（3）High dispersive conductive silver powder is added in organic carrier, mix homogeneously, adds remaining each raw material, disperseed at a high speed,
Send into and mixed on three-roll grinder, ground slurry granularity gets product to 8-15 microns.
It is an advantage of the invention that：
The high dispersive conductive silver powder of the present invention is the surface that nanometer silver powder uniformly and is densely coated on polymer microsphere,
Not only can reduce the consumption of noble metal argentum powder, reduce production cost, at the same also substantially increase nanometer silver powder dispersibility and
Stability；
The organic carrier of the present invention, by adding dispersant, can effectively improve slurry viscosity, improve levelability, make
Obtain slurry to be evenly distributed, argentum powder is with glass dust easily into reunion state.
Specific embodiment
Embodiment 1
A kind of high dispersive conductive silver paste containing chromium, it is characterised in that it is made up of the raw material of following weight parts：
High dispersive conductive silver powder 107, stearic acid monoglyceride 0.6, diethylene glycol ether acetate 30, butanone 4, polyamide
20th, N-Methyl pyrrolidone 0.5, butoxy ethanol 1.3, trioctyl trimellitate (TOTM) 1, chromium methionine 0.2, Diammonium phosphate (DAP) 1, glass
Glass powder 15, calcium acetylacetonate 0.6；
What described high dispersive conductive silver powder was made up of the raw material of following weight parts：
Nano aluminium oxide 10, di-n-octyl sebacate 0.2, deionized water 400, styrene 7, alkylphenol polyoxyethylene 0.8,
Silane coupler KH560 1-2, Ammonium persulfate. 0.02, silver nitrate 140, polyvinylpyrrolidone 1, sodium hypophosphite 40, three (nonylbenzenes
Base) phosphite 3；
Nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 mixing, 700 revs/min of stirrings are mixed 20 minutes,
Add styrene, alkylphenol polyoxyethylene, the 35% of deionized water weight, magnetic agitation 50 minutes, add Ammonium persulfate., surpass
Sound wave shock 15h, obtains nanoemulsions；
Silver nitrate, polyvinylpyrrolidone are mixed, the 50% of remaining deionized water weight is added, is stirred, obtain oxygen
Change liquid；
Remaining each raw material is mixed, Deca ammonia, it is 10.5 to adjust PH, is reducing solution；
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions, stirring reaction 50 minutes, centrifugation are added after completion of dropping
Separate, deionized water and washing with alcohol 3 times, drying are obtained final product.
A kind of preparation method of the high dispersive conductive silver paste containing chromium, it is characterised in that comprise the following steps：
（1）Chromium methionine is added in butoxy ethanol, calcium acetylacetonate is stirring evenly and then adding into, is stirred at 70 DEG C
Mixing 6-10 minutes, obtain dispersant；
（2）Polyamide is added in diethylene glycol ether acetate, trioctyl trimellitate (TOTM), fourth is stirring evenly and then adding into
Ketone, stirring mixing 5 minutes at 80 DEG C add dispersant, 100 revs/min of dispersed with stirring 3 minutes to obtain organic carrier；
（3）High dispersive conductive silver powder is added in organic carrier, mix homogeneously, adds remaining each raw material, disperseed at a high speed,
Send into and mixed on three-roll grinder, ground slurry granularity gets product to 8-15 microns.
Performance test：
After stirring without lump, in uniform state；
Fineness≤15 μm；
Adhesive force 4.6B；
Hardness 1.3H.
Claims (2)
1. a kind of high dispersive conductive silver paste containing chromium, it is characterised in that it is made up of the raw material of following weight parts：High dispersive
Conductive silver powder 100-107, stearic acid monoglyceride 0.4-0.6, diethylene glycol ether acetate 25-30, butanone 4-6, polyamide
14-20, N-Methyl pyrrolidone 0.5-1, butoxy ethanol 1-1.3, trioctyl trimellitate (TOTM) 1-2, chromium methionine 0.1-
0.2nd, Diammonium phosphate (DAP) 1-2, glass dust 10-15, calcium acetylacetonate 0.6-1；Described high dispersive conductive silver powder is by following weight
What the raw material of part was formed：Nano aluminium oxide 5-10, di-n-octyl sebacate 0.1-0.2, deionized water 300-400, styrene 4-7,
It is alkylphenol polyoxyethylene 0.8-1, silane coupler KH560 1-2, Ammonium persulfate. 0.01-0.02, silver nitrate 131-140, poly-
Vinylpyrrolidone 1-2, sodium hypophosphite 30-40, three (nonyl phenyl) phosphite 2-3；
The preparation method of high dispersive conductive silver powder is：
By nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 mixing, 500-700 rev/min of 20-30 point of stirring mixing
Clock, adds styrene, alkylphenol polyoxyethylene, the 30-35% of deionized water weight, magnetic agitation 40-50 minute, adds
Ammonium sulfate, ultrasonic wave concussion 10-15h, obtains nanoemulsions；
Silver nitrate, polyvinylpyrrolidone are mixed, the 40-50% of remaining deionized water weight is added, is stirred, obtain oxygen
Change liquid；
Remaining each raw material is mixed, Deca ammonia, regulation pH is 10-10.5, is reducing solution；
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions, stirring reaction 30-50 minute, centrifugation are added after completion of dropping
Separate, deionized water and washing with alcohol 3-5 time are dried, and are obtained final product.
2. a kind of preparation method of the high dispersive conductive silver paste containing chromium as claimed in claim 1, it is characterised in that including following
Step：
（1）Chromium methionine is added in butoxy ethanol, is stirring evenly and then adding at calcium acetylacetonate, 60-70 DEG C and is stirred
Mixing 6-10 minutes, obtain dispersant；
（2）Polyamide is added in diethylene glycol ether acetate, trioctyl trimellitate (TOTM), butanone is stirring evenly and then adding into,
The stirring mixing 4-5 minutes at 70-80 DEG C, dispersant is added, 60-100 rev/min of dispersed with stirring 3-5 minute, obtain organic carrier；
（3）High dispersive conductive silver powder is added in organic carrier, mix homogeneously, adds remaining each raw material, disperseed at a high speed, sent into
Mixed on three-roll grinder, ground slurry granularity gets product to 8-15 microns.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410775520.XA CN104505151B (en) | 2014-12-16 | 2014-12-16 | Chromium-containing high-dispersity conductive silver paste |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410775520.XA CN104505151B (en) | 2014-12-16 | 2014-12-16 | Chromium-containing high-dispersity conductive silver paste |
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| CN104505151A CN104505151A (en) | 2015-04-08 |
| CN104505151B true CN104505151B (en) | 2017-04-19 |
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| CN105772705A (en) * | 2016-03-22 | 2016-07-20 | 苏州捷德瑞精密机械有限公司 | Conductive silver powder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
| CN103000250A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Back silver paste for low-silver-content crystalline silicon solar battery and preparation method thereof |
| CN103192074A (en) * | 2013-04-10 | 2013-07-10 | 张宇 | Highly dispersed sliver powder and conductive silver paste for film batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5951918A (en) * | 1995-02-08 | 1999-09-14 | Hitachi Chemical Company, Ltd. | Composite electroconductive powder, electroconductive paste, process for producing electroconductive paste, electric circuit and process for producing electric circuit |
| CN103500596B (en) * | 2013-09-30 | 2016-03-23 | 广州市尤特新材料有限公司 | A kind of preparation method of Graphene touch-screen silver slurry |
| CN103980410B (en) * | 2014-04-30 | 2016-02-24 | 中国科学院化学研究所 | A kind of composition and method of making the same for 3D printing and goods |
| CN104078093B (en) * | 2014-06-04 | 2016-09-28 | 乐凯特科技铜陵有限公司 | A kind of high-strength PC B circuit board conductive silver slurry and preparation method thereof |
| CN104143377A (en) * | 2014-06-30 | 2014-11-12 | 永利电子铜陵有限公司 | PCB conductive silver paste and preparing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
| CN103000250A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Back silver paste for low-silver-content crystalline silicon solar battery and preparation method thereof |
| CN103192074A (en) * | 2013-04-10 | 2013-07-10 | 张宇 | Highly dispersed sliver powder and conductive silver paste for film batteries |
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Effective date of registration: 20200921 Address after: Wujiang District of Suzhou City, Jiangsu province 215200 Lili town Yuexiu Road No. 888 Patentee after: Suzhou Yongding Zhilian Technology Co., Ltd Address before: 233122 Anhui city of Chuzhou province Fengyang County town south of Fuxi Patentee before: ANHUI FENGYANG DECHENG TECHNOLOGY Co.,Ltd. |