CN1174827C - Preparation of hexagonal plate silver powder by chemical reduction process - Google Patents
Preparation of hexagonal plate silver powder by chemical reduction process Download PDFInfo
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- CN1174827C CN1174827C CNB01124142XA CN01124142A CN1174827C CN 1174827 C CN1174827 C CN 1174827C CN B01124142X A CNB01124142X A CN B01124142XA CN 01124142 A CN01124142 A CN 01124142A CN 1174827 C CN1174827 C CN 1174827C
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- silver powder
- silver
- powder
- hexagonal plate
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Abstract
The present invention provides a new technology for preparing silver powder with different patterns by using a chemical reduction method. Silver nitrate is used as a predecessor, and hydrogen peroxide is used as a reducing agent; dispersed spherical or flaky hexagonal silver powder can be obtained through synthesis under the condition that a protecting agent, a disperser PVP (kollidon), catalyst-Chloroplatinic acid exist in the mixed media of alcohol (ethylene glycol, ethanol) and water. The granularity of the obtained spherical silver powder is less than 0.5 micrometre. The flaky hexagonal silver powder is well developed silvery white monocrystal powder, and has the maximum size of 30 to 50 micrometres and has the thickness of 0.1 to 0.5 micrometre.
Description
1. technical field:
Invention belongs to the metal powder material preparation field
2. background technology:
The silver slurry is the most important material of electronics industry, silver powder as silver slurry filler, it then is critical material, requirement to it should be pure, thin again, also want good dispersion, and its coating of particles is had higher and special requirement, the spherical powder that people know has maximum specific surface and higher surface energy (activity), comparatively speaking, its oxidizability and oxidation potential are higher.What its conductibility in conductive layer relied on is intergranular some contact, therefore has the shortcoming of high electrical resistance and poorly conductive.And flake silver powder is just the opposite, the specific area of particle is less relatively, specific surface energy is lower, and stable, oxidizability and oxidation potential are lower, intergranular contact is face or line, resistance is relatively low, and electric conductivity is preferably arranged, and increases and guarantee the reliability of electronic devices and components like this, can also reduce simultaneously the thickness of coating, for miniaturization provides advantage.Prove in the practice that the coating of flaky powder preparation has higher electric conductivity.
At present, prepare flake silver powder in the world, the overwhelming majority at first utilizes chemistry or physical method to make spherical or dendritic silver powder, makes it slabbing through pulverizing with grinding for a long time then.These class methods not only operation are many, and the energy consumption height, the more important thing is that powder is easily polluted by process and medium.Simultaneously, under the mechanical force, can cause the sclerosis of silver powder for a long time, influence the result of use of silver powder.Also once the someone manufactures experimently out flake silver powder, but used reagent has bigger toxicity, is benzaldehyde as the used reducing agent of United States Patent (USP) U.S.Pat 447674 and China Central South University, has cyanide to produce in the process, not only process condition is abominable, and causes environmental pollution.
3. summary of the invention
The object of the invention is to utilize nontoxic chemical reagent, adopts simple method, and a step directly prepares the hexagonal plate silver powder of providing satisfactory electrical conductivity.
Under the normal pressure, with glassware as reaction vessel, with alcohol-ammonia as medium, silver nitrate is a predecessor, hydrogen peroxide is a reducing agent, and chloroplatinic acid is a catalyst, is being added with under the condition of polyvinylpyrrolidone as dispersant, by the ratio of control component, can obtain the silver powder of hexagonal flake effectively.Chloroplatinic acid is as catalyst, and its scope is that the mol ratio of platinum and silver is 1 * 10
-4～5 * 10
-3, silver concentration is 0.01～0.15mol/L, and ammonia is 2.0～5.0 with the mol ratio of silver, and reaction temperature is 10～80 ℃ under the normal pressure, 300～1200 rev/mins of mixing speeds, adding reducing agent afterreaction is finished in 5 minutes～3 hours.
According to method of the present invention, can a step prepare silvery white glittering monodispersed hexagonal plate silver powder crystal, particle size 0.1～100 μ effectively
m, thickness is≤0.5 μ
m
With the prepared silver powder electron scanning micrograph of the present invention, see Fig. 1-3.
4. description of drawings
The electron scanning photo of the hexagonal flake powder silver that Fig. 1 makes for ethylene glycol-ammono-system;
Fig. 2 is the hexagonal plate silver powder electron scanning photo that ethylene glycol-ammonia-aqueous systems makes;
The electron scanning photo of the near-spherical silver powder that Fig. 3 makes for ethylene glycol-ammono-system.
5. the specific embodiment
Embodiment 1: in the beaker that 150ml ethylene glycol is arranged, add silver nitrate 2.123g, stir down, adding concentration is 28% ammoniacal liquor 5.08ml, adds polyethylene of dispersing agent pyrrolidones 2.13 grams then, adding concentration again is the chloroplatinic acid 4.8ml of 5g/L, add concentration at last and be 30% hydrogen peroxide 6.4ml, stirring reaction separated after 2 hours, with distilled water and acetone washing, drying at room temperature four hours, gained powder are surveyed and are shown and check.(see figure 1)
Embodiment 2: 75ml ethanol and 75ml distilled water are added in the beaker, and other is done as example 1, also obtains same flake silver powder at last.(see figure 2)
Embodiment 3: in 150ml ethylene glycol, add silver nitrate 2.123g, and ammoniacal liquor 2.54ml, 30% hydrogen peroxide 1.28ml, the chloroplatinic acid 0.07ml of concentration 5g/L, polyvinylpyrrolidone 2.123g reacts and obtains near-spherical silver powder after 2 hours.(see figure 3)
Claims (1)
1. method for preparing hexagonal plate silver powder, this method adopts the mixed system of the ethylene glycol, ethanol, glycerine of silver nitrate or itself and water, it is characterized in that preparing the alcoholic solution of 0.01～0.15mol/L silver nitrate, it is short molten to add concentration and be 28% ammoniacal liquor, the mol ratio of control ammonia and silver ion is 2.0～5.0: 1, and adding the catalyst chloroplatinic acid, the mol ratio of control platinum ion and silver ion is 1 * 10
-4～5 * 10
-3: 1, adding is as the polyvinylpyrrolidone of dispersant, its addition is that the mass ratio of polyvinylpyrrolidone and silver ion is 1: 1, adding concentration is 30% hydrogenperoxide steam generator, and addition is controlled at the mol ratio of hydrogen peroxide and silver ion between 6: 1, and the reaction time is 5 minutes to 2 hours, produce silvery white precipitation, after liquid-solid separation, washing, normal temperature～60 ℃ drying obtains the hexagonal plate silver powder of silvery white good dispersion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01124142XA CN1174827C (en) | 2001-08-17 | 2001-08-17 | Preparation of hexagonal plate silver powder by chemical reduction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01124142XA CN1174827C (en) | 2001-08-17 | 2001-08-17 | Preparation of hexagonal plate silver powder by chemical reduction process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1401452A CN1401452A (en) | 2003-03-12 |
| CN1174827C true CN1174827C (en) | 2004-11-10 |
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|---|---|---|---|
| CNB01124142XA Expired - Fee Related CN1174827C (en) | 2001-08-17 | 2001-08-17 | Preparation of hexagonal plate silver powder by chemical reduction process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431752C (en) * | 2006-09-30 | 2008-11-12 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
Families Citing this family (11)
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|---|---|---|---|---|
| JP4489388B2 (en) * | 2003-07-29 | 2010-06-23 | 三井金属鉱業株式会社 | Method for producing fine silver powder |
| JP4320447B2 (en) * | 2004-02-03 | 2009-08-26 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder and method for producing the same |
| US7648557B2 (en) * | 2006-06-02 | 2010-01-19 | E. I. Du Pont De Nemours And Company | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom |
| CN100531975C (en) * | 2006-12-14 | 2009-08-26 | 中国科学院理化技术研究所 | Chemical preparing process for flake micron silver powder |
| CN102254702A (en) * | 2011-04-12 | 2011-11-23 | 常州大学 | Composite light anode material and application thereof to dye sensitized cell preparation |
| CN103831444B (en) * | 2014-03-11 | 2015-12-02 | 上海交通大学 | A kind of preparation method of high crystallization flake silver powder |
| KR101618093B1 (en) * | 2014-03-17 | 2016-05-09 | 주식회사 상보 | A Conductive Paste Composition for Forming Conductive Thin Film on a Flexible Substrate and a method for producing the same |
| CN110919025B (en) * | 2019-12-04 | 2022-08-30 | 郴州市金贵银业股份有限公司 | Preparation method of nano paillette silver powder |
| CN110899722B (en) * | 2019-12-26 | 2022-07-01 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
| CN111451521B (en) * | 2020-03-30 | 2022-06-03 | 长春黄金研究院有限公司 | Method for preparing high-tap-density spherical silver powder by chemical method |
| CN111992734B (en) * | 2020-08-21 | 2022-02-22 | 山东建邦胶体材料有限公司 | Preparation method of nano-silver with controllable particle size |
-
2001
- 2001-08-17 CN CNB01124142XA patent/CN1174827C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431752C (en) * | 2006-09-30 | 2008-11-12 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
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| CN1401452A (en) | 2003-03-12 |
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