CN103433502A - High-dispersing silver powder and preparation method thereof - Google Patents
High-dispersing silver powder and preparation method thereof Download PDFInfo
- Publication number
- CN103433502A CN103433502A CN2013103499746A CN201310349974A CN103433502A CN 103433502 A CN103433502 A CN 103433502A CN 2013103499746 A CN2013103499746 A CN 2013103499746A CN 201310349974 A CN201310349974 A CN 201310349974A CN 103433502 A CN103433502 A CN 103433502A
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- Prior art keywords
- epoxy resin
- bisphenol
- type epoxy
- silver powder
- nano
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000003822 epoxy resin Substances 0.000 claims abstract description 45
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 45
- 239000006185 dispersion Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- -1 polyethylene Polymers 0.000 claims description 7
- 229920000573 polyethylene Polymers 0.000 claims description 7
- 150000004040 pyrrolidinones Chemical class 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000012856 packing Methods 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses high-dispersing silver powder and a preparation method thereof. The high-dispersing silver powder is formed by 25-35% of bisphenol A type epoxy resin and 65-75% nano-silver layer coated at the face of the biphenol A type epoxy resin according to mass percent. The in-situ synthesized silver powder can be uniformly and compactly coated at the face of the biphenol A type epoxy resin, thus improving the dispersing stability of the nano-silver powder, reducing the use level of valuable metal silver powder and reducing the production cost; meanwhile, the high-dispersing silver powder is adopted as a conductive packing in conductive silver slurry, so higher conductivity can be realized under the condition of lower silver powder use level.
Description
Technical field
The invention belongs to the photovoltaic material preparing technical field, particularly a kind of high dispersive type silver powder and preparation method thereof.
Background technology
Silver powder and electric slurry thereof are a kind of noble metal powders be most widely used in electronics industry with the consumption maximum, are the key function materials of producing various electronic component products.The dispersion of silver powder in conductive silver paste is very important.Because the particle diameter of nano-silver powder is less, apparent activation energy is higher, the difficult dispersion, agglomeration easily occurs.
Therefore, how to improve the dispersion stabilization of nano-silver powder in the silver slurry is the focus of research always.Chinese patent (CN 101003907 B) discloses a kind of preparation method of metal and dielectric composite grains of silicon dioxide coated by Nano silver, it adopts ultrasonic electrochemical method one step Nano silver grain to be deposited to the surface of silica spheres, and its surface distributed is very even, there is prospects for commercial application preferably.
The present invention is coated on the bisphenol A type epoxy resin surface by original position synthesis of nano silver layer, can improve the dispersiveness of nano-silver powder in the silver slurry.
Summary of the invention
The present invention is directed to nano-silver powder in prior art exists the problem of easy reunion, bad dispersibility and a kind of high dispersive type silver powder is provided in the silver slurry.
Purpose of the present invention is achieved through the following technical solutions:
A kind of high dispersive type silver powder, by bisphenol A type epoxy resin and the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, formed, it is characterized in that: by bisphenol A type epoxy resin and the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, formed, press the mass percent ratio, described bisphenol A type epoxy resin accounts for 25～35%, nano-silver layer accounts for 65～75%.
Another object of the present invention is to provide a kind of method for preparing above-mentioned high dispersive type silver powder.
A kind of preparation method of high dispersive type silver powder, its concrete preparation process is: bisphenol A type epoxy resin is mixed with to 40%～60% bisphenol A type epoxy resin dispersion liquid, the liquor argenti nitratis ophthalmicus and the polyethylene of dispersing agent pyrrolidones that add 2mol/L, stir, be warming up to 40 ℃～60 ℃, then the reducing agent hydrazine hydrate solution that adds 0.5mol/L, under stirring condition, reaction 30～50min, the ammonia spirit regulation system pH value that is 2%～5% with mass fraction is 5～6, after completion of the reaction, product is through centrifugation, and wash 3～5 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, obtain high dispersive type silver powder, wherein the mass ratio of liquor argenti nitratis ophthalmicus and bisphenol A type epoxy resin dispersion liquid is 1～3:1, the mass ratio of polyvinylpyrrolidone and bisphenol A type epoxy resin dispersion liquid is 0.05～0.2:1, the mass ratio of hydrazine hydrate solution and liquor argenti nitratis ophthalmicus is 0.1～0.5:1.
Remarkable advantage of the present invention is:
But 1, be coated on the bisphenol A type epoxy resin surface the present invention's nano-silver powder even compact synthetic by original position, improved dispersiveness and the stability of nano-silver powder, reduce the consumption of noble metal silver powder, reduce production costs.
2, the present invention adopts high dispersive type silver powder as the conductive filler in conductive silver paste, can make in the situation that the silver powder consumption is lower, realizes higher conductance.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
50 gram bisphenol A type epoxy resin E44 are dissolved in the mixed solvent of 300 gram toluene and butanone, toluene 200 grams wherein, butanone 100 grams, stir, make bisphenol A type epoxy resin E44 dispersion liquid, the liquor argenti nitratis ophthalmicus and the 2.5 gram polyethylene of dispersing agent pyrrolidones that add 50 gram 2mol/L, stir, be warming up to 40 ℃, then the hydrazine hydrate solution that adds 5 gram 0.5mol/L, under stirring condition, react 30 minutes, the ammonia spirit regulation system pH value that is 2% with mass fraction is 5, after completion of the reaction, product is through centrifugation, and wash 3 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on bisphenol A type epoxy resin E44 surface, obtain high dispersive type silver powder.
Embodiment 2
50 gram bisphenol A type epoxy resin E51 are dissolved in the mixed solvent of 600 gram toluene and butanone, toluene 400 grams wherein, butanone 200 grams, stir; Make bisphenol A type epoxy resin E51 dispersion liquid, the liquor argenti nitratis ophthalmicus and the 10 gram polyethylene of dispersing agent pyrrolidones that add 150 gram 2mol/L, stir, be warming up to 60 ℃, then the hydrazine hydrate solution that adds 7.5 gram 0.5mol/L, under stirring condition, react 50 minutes, the ammonia spirit regulation system pH value that is 5% with mass fraction is 6, and after completion of the reaction, product is through centrifugation, and wash 3 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on bisphenol A type epoxy resin E51, obtain high dispersive type silver powder.
Embodiment 3
50 gram bisphenol A type epoxy resin E55 are dissolved in the mixed solvent of 450 gram toluene and butanone, toluene 300 grams wherein, butanone 150 grams, stir; Make bisphenol A type epoxy resin E55 dispersion liquid, the liquor argenti nitratis ophthalmicus and the 5 gram polyethylene of dispersing agent pyrrolidones that add 100 gram 2mol/L, stir, be warming up to 60 ℃, then the hydrazine hydrate solution that adds 25 gram 0.5mol/L, under stirring condition, react 50 minutes, the ammonia spirit regulation system pH value that is 3% with mass fraction is 6, and after completion of the reaction, product is through centrifugation, and wash 4 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on bisphenol A type epoxy resin E55 surface, obtain high dispersive type silver powder.
Claims (5)
1. a high dispersive type silver powder is characterized in that: be comprised of bisphenol A type epoxy resin and the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, press the mass percent ratio, described bisphenol A type epoxy resin accounts for 25～35%, nano-silver layer accounts for 65～75%.
2. high dispersive type silver powder according to claim 1, it is characterized in that: described nano-silver layer is by liquor argenti nitratis ophthalmicus, the polyethylene of dispersing agent pyrrolidones synthesizes and makes through reducing agent hydrazine hydrate solution original position, its concrete preparation process is: bisphenol A type epoxy resin is mixed with to 40%～60% bisphenol A type epoxy resin dispersion liquid, the liquor argenti nitratis ophthalmicus and the polyethylene of dispersing agent pyrrolidones that add 2mol/L, stir, be warming up to 40 ℃～60 ℃, then the reducing agent hydrazine hydrate solution that adds 0.5mol/L, under stirring condition, reaction 30～50min, the ammonia spirit regulation system pH value that is 2%～5% with mass fraction is 5～6, after completion of the reaction, product is through centrifugation, and wash 3～5 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, obtain high dispersive type silver powder, wherein the mass ratio of liquor argenti nitratis ophthalmicus and bisphenol A type epoxy resin dispersion liquid is 1～3:1, the mass ratio of polyvinylpyrrolidone and bisphenol A type epoxy resin dispersion liquid is 0.05～0.2:1, the mass ratio of hydrazine hydrate solution and liquor argenti nitratis ophthalmicus is 0.1～0.5:1.
3. high dispersive type silver powder according to claim 1 and 2, it is characterized in that: described bisphenol A type epoxy resin is bisphenol A type epoxy resin E44, bisphenol A type epoxy resin E51 or bisphenol A type epoxy resin E55.
4. a method for preparing high dispersive type silver powder as claimed in claim 1, it is characterized in that: bisphenol A type epoxy resin is mixed with to 40%～60% bisphenol A type epoxy resin dispersion liquid, the liquor argenti nitratis ophthalmicus and the polyethylene of dispersing agent pyrrolidones that add 2mol/L, stir, be warming up to 40 ℃～60 ℃, then the reducing agent hydrazine hydrate solution that adds 0.5mol/L, under stirring condition, reaction 30～50min, the ammonia spirit regulation system pH value that is 2%～5% with mass fraction is 5～6, after completion of the reaction, product is through centrifugation, and wash 3～5 times with deionized water and ethanol, dry, prepare the nano-silver layer that is coated on the bisphenol A type epoxy resin surface, obtain high dispersive type silver powder, wherein the mass ratio of liquor argenti nitratis ophthalmicus and bisphenol A type epoxy resin dispersion liquid is 1～3:1, the mass ratio of polyvinylpyrrolidone and bisphenol A type epoxy resin dispersion liquid is 0.05～0.2:1, the mass ratio of hydrazine hydrate solution and liquor argenti nitratis ophthalmicus is 0.1～0.5:1.
5. the preparation method of a kind of high dispersive type silver powder according to claim 4, it is characterized in that: described bisphenol A type epoxy resin is bisphenol A type epoxy resin E44, bisphenol A type epoxy resin E51 or bisphenol A type epoxy resin E55.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103499746A CN103433502A (en) | 2013-08-13 | 2013-08-13 | High-dispersing silver powder and preparation method thereof |
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| CN2013103499746A CN103433502A (en) | 2013-08-13 | 2013-08-13 | High-dispersing silver powder and preparation method thereof |
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| CN103433502A true CN103433502A (en) | 2013-12-11 |
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| CN2013103499746A Pending CN103433502A (en) | 2013-08-13 | 2013-08-13 | High-dispersing silver powder and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980665A (en) * | 2014-05-19 | 2014-08-13 | 上海维度化工科技有限公司 | Waterborne antibacterial composite material and preparation method thereof |
| CN104505142A (en) * | 2014-12-16 | 2015-04-08 | 安徽凤阳德诚科技有限公司 | Conductive silver paste |
| CN105665745A (en) * | 2016-04-10 | 2016-06-15 | 欧振云 | Preparation method of silver nanoparticles |
| CN106165024A (en) * | 2014-03-28 | 2016-11-23 | 三菱综合材料株式会社 | Conductive paste |
| CN109692971A (en) * | 2018-12-10 | 2019-04-30 | 太原氦舶新材料有限责任公司 | A kind of nano-silver powder and its preparation and the application in low-temperature cured conductive silver paste |
| CN114181586A (en) * | 2021-11-26 | 2022-03-15 | 洛阳双瑞防腐工程技术有限公司 | Water-based epoxy static-conducting oil-resistant anticorrosive paint and preparation method thereof |
| CN115673334A (en) * | 2022-10-26 | 2023-02-03 | 陕西煤业化工技术研究院有限责任公司 | Micro-nano silver dispersion and preparation method thereof |
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| CN1939999A (en) * | 2005-09-27 | 2007-04-04 | 上海特视精密仪器有限公司 | Sliver-powder conducting glue and its production |
| CN101215450A (en) * | 2008-01-08 | 2008-07-09 | 上海大学 | Conductive adhesive added with short rod-shaped nano-silver powder and preparation method thereof |
| CN101569937A (en) * | 2009-06-05 | 2009-11-04 | 中国乐凯胶片集团公司 | Preparation method for high-dispersing silver powder used for conductive silver paste |
| CN102634312A (en) * | 2012-03-27 | 2012-08-15 | 烟台德邦电子材料有限公司 | Silvering powder conductive adhesive for LED packaging and production method thereof |
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- 2013-08-13 CN CN2013103499746A patent/CN103433502A/en active Pending
Patent Citations (5)
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| CN1939999A (en) * | 2005-09-27 | 2007-04-04 | 上海特视精密仪器有限公司 | Sliver-powder conducting glue and its production |
| CN101215450A (en) * | 2008-01-08 | 2008-07-09 | 上海大学 | Conductive adhesive added with short rod-shaped nano-silver powder and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106165024A (en) * | 2014-03-28 | 2016-11-23 | 三菱综合材料株式会社 | Conductive paste |
| US10332649B2 (en) | 2014-03-28 | 2019-06-25 | Mitsubishi Materials Corporation | Conductive paste |
| CN103980665A (en) * | 2014-05-19 | 2014-08-13 | 上海维度化工科技有限公司 | Waterborne antibacterial composite material and preparation method thereof |
| CN104505142A (en) * | 2014-12-16 | 2015-04-08 | 安徽凤阳德诚科技有限公司 | Conductive silver paste |
| CN105665745A (en) * | 2016-04-10 | 2016-06-15 | 欧振云 | Preparation method of silver nanoparticles |
| CN109692971A (en) * | 2018-12-10 | 2019-04-30 | 太原氦舶新材料有限责任公司 | A kind of nano-silver powder and its preparation and the application in low-temperature cured conductive silver paste |
| CN114181586A (en) * | 2021-11-26 | 2022-03-15 | 洛阳双瑞防腐工程技术有限公司 | Water-based epoxy static-conducting oil-resistant anticorrosive paint and preparation method thereof |
| CN115673334A (en) * | 2022-10-26 | 2023-02-03 | 陕西煤业化工技术研究院有限责任公司 | Micro-nano silver dispersion and preparation method thereof |
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Application publication date: 20131211 |