CN103737011B - The preparation method of high compaction spherical silver powder - Google Patents
The preparation method of high compaction spherical silver powder Download PDFInfo
- Publication number
- CN103737011B CN103737011B CN201310137872.8A CN201310137872A CN103737011B CN 103737011 B CN103737011 B CN 103737011B CN 201310137872 A CN201310137872 A CN 201310137872A CN 103737011 B CN103737011 B CN 103737011B
- Authority
- CN
- China
- Prior art keywords
- silver powder
- argenti nitratis
- nitratis ophthalmicus
- liquor argenti
- high compaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of high compaction spherical silver powder, comprise the following steps: 1. prepare liquor argenti nitratis ophthalmicus and reductant solution respectively, liquor argenti nitratis ophthalmicus concentration is 1-50g/L, liquor argenti nitratis ophthalmicus and reductant solution at 1-250g/L, and all cool to 0-20 DEG C by reductant solution concentration; 2. in liquor argenti nitratis ophthalmicus, add macromolecule dispersant and complexing agent, mix; 3. under agitation, step is joined 3. in gained liquor argenti nitratis ophthalmicus by disposable for reducing agent; 4. above-mentioned solution is constantly stirred, until solution colour no longer changes, then after centrifugation or natural subsidence, first spends deionized water for several times, then with absolute ethanol washing for several times; 5. vacuum drying under 50-80 DEG C of condition, obtains the high compaction spherical silver powder of particle diameter 1-3 μm of scope.The preparation method of high compaction spherical silver powder of the present invention can not only realize batch production, and the silver powder prepared is that particle diameter is ultra-fine, distributes, and have good sphericity and comparatively smooth surface in the scope of 1-3 μm very narrow.
Description
Technical field
The present invention relates to a kind of preparation method of silver powder, particularly relate to a kind of preparation method of high compaction spherical silver powder.
Background technology
Silver slurry is the most important material of electronics industry, along with the microminiaturization of electronic product and the development of micro & nano technology, various conductive paste and thick film ink is prepared, on the coating being widely used in printed circuit and circuit interconnection with powder (especially silver powder).Especially in recent years the development rapidly of photovoltaic industry, has higher requirement to silver powder, and it is large that it requires that silver powder has tap density, the features such as good dispersion.Preparing silver powder both at home and abroad has a lot of method, as thermal decomposition method, electrochemical process, aeroponics, wet chemistry method etc. at present.Wherein to have production technology simple for wet chemistry method, the advantages such as size tunable and attention.Prepare in ball shape silver powder at wet chemistry method, generally all with AgNO3, Ag2CO3, [Ag (NH3) 2]
+and other compounds of silver are as silver-colored source, reducing agent also has a lot, as formaldehyde, and formates, hydrazine hydrate, glucose, polyalcohol, ferrous salt, ascorbic acid etc.Control silver powder particle diameter to control reaction speed to realize, a lot of people has done a lot of work, and the patent being CN1106326A as publication number adopts alkanolamine to serve as complexing agent, under PH cushioning liquid exists, temperature, when 10-100 DEG C, is reacted, and generates dense packing, spherical shaped spherical powder particle.But the method reagent dosage is comparatively large, process is complicated, particle size distribution range is wider, silver powder tap density is large not.And the patent that publication number is CN1266761A adopts polyvinylpyrrolidone (PVP), alkyl hydrosulfide (RSH) etc. as the protective agent of galactic nucleus growth course, ammoniacal liquor serves as complexing agent, and Vc is as reducing agent.This patent silver nitrate is made into silver ammino solution as silver-colored source, then adds reducing agent and prepare silver powder.Although obtained silver powder has the advantage such as stability, good dispersion, be not suitable for suitability for industrialized production.Publication number is that the patent of CN1387968A then adopts carbonate to serve as complexing agent, surfactant is that protective agent is to prepare silver powder.Although the silver powder sphericity that the method is produced is better, complex steps, does not have industrial prospect.CN1327521A also adopts ferric sulfate direct-reduction silver nitrate can prepare uniform ball shape silver powder in addition, but silver powder surface is smooth not, and upside-down mounting tap density is large not.
Summary of the invention
In order to overcome above-mentioned defect, the invention provides a kind of preparation method of high compaction spherical silver powder, the method can not only realize batch production, and the silver powder prepared is that particle diameter is ultra-fine, distribute in the scope of 1-3 μm very narrow, and there is good sphericity and comparatively smooth surface.
The present invention in order to the technical scheme solving its technical problem and adopt is: a kind of preparation method of high compaction spherical silver powder, comprises the following steps:
1. prepare liquor argenti nitratis ophthalmicus and reductant solution respectively, liquor argenti nitratis ophthalmicus concentration is 1-50g/L, and liquor argenti nitratis ophthalmicus and reductant solution at 1-250g/L, and all cool to 0-20 DEG C by reductant solution concentration;
2. in described liquor argenti nitratis ophthalmicus, add macromolecule dispersant and complexing agent, mix;
3. under agitation, step is joined 3. in gained liquor argenti nitratis ophthalmicus by disposable for described reducing agent;
4. above-mentioned solution is constantly stirred, until solution colour no longer changes, then after centrifugation or natural subsidence, first spends deionized water for several times, then with absolute ethanol washing for several times;
5. vacuum drying under 50-80 DEG C of condition, obtains the high compaction spherical silver powder of particle diameter 1-3 μm of scope.
As preferred version of the present invention, described macromolecule dispersant be at least polyvinylpyrrolidone, 1-METHYLPYRROLIDONE and polyvinyl alcohol one of them.
As preferred version of the present invention, its concentration of described macromolecule dispersant is 0.05-5g/L.
As preferred version of the present invention, described complexing agent be with the organic acid of two carboxyls and plural carboxyl or acid anhydrides one of them.
As preferred version of the present invention, described complexing agent be phthalic acid and this dicarboxylic acid anhydride adjacent one of them.
As preferred version of the present invention, described step 4. in, the mass ratio of described reducing agent and silver nitrate is 2-5.
As preferred version of the present invention, described reducing agent is ascorbic acid (vitamin C is called for short Vc).
The invention has the beneficial effects as follows: 1. adopt silver nitrate as silver-colored source solution, binary or the above organic acid of binary or acid anhydrides are complexing agent; 2. there is technique simple, easy to operate, reproducible, non-environmental-pollution advantage; 3. according to different customer requirement, 1-3 μm of different-grain diameter can be produced and obtain spherical powder; 4. produced ball shape silver powder has the feature of good sphericity and comparatively smooth surface, good dispersion, purity high (>=99.5%), the ideal material producing various thick-film electronic slip, electronics adhesive, as anisotropic conducting resinl/film.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 1 obtains;
Fig. 2 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 2 obtains;
Fig. 3 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 3 obtains;
Fig. 4 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 4 obtains;
Fig. 5 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 5 obtains;
Fig. 6 is the shape appearance figure of silver powder SEM × 1000 that the embodiment of the present invention 6 obtains;
Detailed description of the invention
By reference to the accompanying drawings, elaborate to the present invention, but protection scope of the present invention is not limited to following embodiment, the simple equivalence namely in every case done with the present patent application the scope of the claims and description changes and modifies, and all still belongs within patent covering scope of the present invention.
Embodiment 1:
First prepare liquor argenti nitratis ophthalmicus and reductant solution: take 1g silver nitrate deionized water dissolving constant volume in 50ml (20g/L), add phthalic acid 0.1g, add PVP solution (10%) 2ml, take 2.3gVc deionized water dissolving constant volume in 50ml (46g/L).Both are all cooled to 15 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 50 DEG C, vacuum drying obtains silver powder.As shown in Figure 1, have better sphericity, average grain diameter is 1.5 μm to gained silver powder, good dispersion, and domain size distribution is narrower, and purity is high, tap density 4.7g/cm
3.
Embodiment 2:
Prepare liquor argenti nitratis ophthalmicus and reductant solution: take 2g silver nitrate deionized water dissolving constant volume in 50ml (40g/L), add tartaric acid 0.05g, add 1-METHYLPYRROLIDONE 2ml; Take 5gVc deionized water dissolving constant volume again in 50ml (100g/L).Both are all cooled to 8 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 65 DEG C, vacuum drying obtains silver powder.As shown in Figure 2, have better sphericity, average grain diameter is 3.0 μm to gained silver powder, and good dispersion, purity is high.Tap density 4.5g/cm
3.
Embodiment 3:
First prepare liquor argenti nitratis ophthalmicus and reductant solution: take 1.275g silver nitrate deionized water dissolving constant volume in 50ml (25.5g/L), add phthalic acid 0.1g, add PVP solution (10%) 2ml, take 5.1gVc deionized water dissolving constant volume in 50ml (102g/L).Both are all cooled to 20 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 50 DEG C, vacuum drying obtains silver powder.As shown in Figure 3, have better sphericity, average grain diameter is 1.0 μm to gained silver powder, good dispersion, and domain size distribution is narrower, and purity is high, tap density 4.8g/cm
3.
Embodiment 4:
First prepare liquor argenti nitratis ophthalmicus and reductant solution: take 1.5g silver nitrate deionized water dissolving constant volume in 50ml (30g/L), add phthalic acid 0.1g, add PVP solution (10%) 2ml, take 3gVc deionized water dissolving constant volume in 50ml (60g/L).Both are all cooled to 0 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 60 DEG C, vacuum drying obtains silver powder.As shown in Figure 4, have better sphericity, average grain diameter is 2.0 μm to gained silver powder, good dispersion, and domain size distribution is narrower, and purity is high, tap density 4.6g/cm
3.
Embodiment 5:
First prepare liquor argenti nitratis ophthalmicus and reductant solution: take 0.5g silver nitrate deionized water dissolving constant volume in 50ml (10g/L), add phthalic acid 0.1g, add PVP solution (10%) 2ml, take 2.5gVc deionized water dissolving constant volume in 50ml (50g/L).Both are all cooled to 10 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 70 DEG C, vacuum drying obtains silver powder.As shown in Figure 5, have better sphericity, average grain diameter is 2.7 μm to gained silver powder, good dispersion, and domain size distribution is narrower, and purity is high, tap density 4.4g/cm
3.
Embodiment 6:
First prepare liquor argenti nitratis ophthalmicus and reductant solution: take 0.05g silver nitrate deionized water dissolving constant volume in 50ml (1g/L), add phthalic acid 0.1g, add PVP solution (10%) 2ml, take 0.25gVc deionized water dissolving constant volume in 50ml (4.5g/L).Both are all cooled to 5 DEG C.Then under agitation both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, spends deionized water 3 times, and then use absolute ethanol washing 2 times, at 80 DEG C, vacuum drying obtains silver powder.As shown in Figure 6, have better sphericity, average grain diameter is 3.0 μm to gained silver powder, good dispersion, and domain size distribution is narrower, and purity is high, tap density 4.3g/cm
3.
Claims (5)
1. a preparation method for high compaction spherical silver powder, is characterized in that comprising the following steps:
1. prepare liquor argenti nitratis ophthalmicus and reductant solution respectively, liquor argenti nitratis ophthalmicus concentration is 1-50g/L, and liquor argenti nitratis ophthalmicus and reductant solution at 1-250g/L, and all cool to 0-20 DEG C by reductant solution concentration;
2. in described liquor argenti nitratis ophthalmicus, add macromolecule dispersant and complexing agent, mix;
3. under agitation, step is joined 3. in gained liquor argenti nitratis ophthalmicus by disposable for described reducing agent;
4. above-mentioned solution is constantly stirred, until solution colour no longer changes, then after centrifugation or natural subsidence, first spends deionized water for several times, then with absolute ethanol washing for several times;
5. vacuum drying under 50-80 DEG C of condition, obtains the high compaction spherical silver powder of particle diameter 1-3 μm of scope;
Wherein, described complexing agent be phthalic acid and this dicarboxylic acid anhydride adjacent one of them.
2. the preparation method of high compaction spherical silver powder according to claim 1, is characterized in that: described macromolecule dispersant be at least polyvinylpyrrolidone, 1-METHYLPYRROLIDONE and polyvinyl alcohol one of them.
3. the preparation method of high compaction spherical silver powder according to claim 2, is characterized in that: its concentration of described macromolecule dispersant is 0.05-5g/L.
4. the preparation method of high compaction spherical silver powder according to claim 1, is characterized in that: described step 4. in, the mass ratio of described reducing agent and silver nitrate is 2-5.
5. the preparation method of high compaction spherical silver powder according to claim 1, is characterized in that: described reducing agent is ascorbic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310137872.8A CN103737011B (en) | 2013-04-22 | 2013-04-22 | The preparation method of high compaction spherical silver powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310137872.8A CN103737011B (en) | 2013-04-22 | 2013-04-22 | The preparation method of high compaction spherical silver powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103737011A CN103737011A (en) | 2014-04-23 |
| CN103737011B true CN103737011B (en) | 2016-02-24 |
Family
ID=50494118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310137872.8A Expired - Fee Related CN103737011B (en) | 2013-04-22 | 2013-04-22 | The preparation method of high compaction spherical silver powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103737011B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105583407A (en) * | 2014-11-14 | 2016-05-18 | 中国振华集团云科电子有限公司 | Preparation method of single-dispersion and high-tap-density spherical silver powder |
| CN106270545A (en) * | 2015-06-12 | 2017-01-04 | 中国振华集团云科电子有限公司 | A kind of high-tap density noble metal raw powder's production technology |
| CN111992733A (en) * | 2020-08-06 | 2020-11-27 | 超威电源集团有限公司 | Silver nano catalyst for aluminum air battery and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1387968A (en) * | 2001-05-26 | 2003-01-01 | 西北稀有金属材料研究院 | Prepn of superfine spherical silver powder |
| CN1700360B (en) * | 2004-05-19 | 2010-10-06 | 同和控股（集团）有限公司 | Spherical silver powder and method for producing same |
| CN102343441A (en) * | 2011-09-22 | 2012-02-08 | 上海交通大学 | Method for preparing monodispersed silver powder with high tap density and low agglomeration |
| CN102413967A (en) * | 2009-05-01 | 2012-04-11 | E.I.内穆尔杜邦公司 | Silver particles and a process for making them |
| CN102632248A (en) * | 2012-05-03 | 2012-08-15 | 中国人民解放军国防科学技术大学 | Spherical silver powder and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5415708B2 (en) * | 2008-03-26 | 2014-02-12 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder manufacturing method |
-
2013
- 2013-04-22 CN CN201310137872.8A patent/CN103737011B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1387968A (en) * | 2001-05-26 | 2003-01-01 | 西北稀有金属材料研究院 | Prepn of superfine spherical silver powder |
| CN1700360B (en) * | 2004-05-19 | 2010-10-06 | 同和控股（集团）有限公司 | Spherical silver powder and method for producing same |
| CN102413967A (en) * | 2009-05-01 | 2012-04-11 | E.I.内穆尔杜邦公司 | Silver particles and a process for making them |
| CN102343441A (en) * | 2011-09-22 | 2012-02-08 | 上海交通大学 | Method for preparing monodispersed silver powder with high tap density and low agglomeration |
| CN102632248A (en) * | 2012-05-03 | 2012-08-15 | 中国人民解放军国防科学技术大学 | Spherical silver powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 化学还原法中制备条件对超细银粉形貌的影响;敖毅伟等;《粉末冶金技术》;20071031;第25卷(第05期);355-359 * |
| 球形纳米银粉的制备研究;宋永辉等;《稀有金属材料与工程》;20070430;第36卷(第04期);709-712 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103737011A (en) | 2014-04-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101554664B (en) | Method for preparing nano-scale silver powder | |
| CN101880493B (en) | Method for preparing nano copper conductive ink | |
| US8231704B2 (en) | Silver particles and processes for making them | |
| US8372178B2 (en) | Silver particles and processes for making them | |
| US8366799B2 (en) | Silver particles and a process for making them | |
| CN104096850B (en) | The method that silver ammonia complex prepares superfine spherical silver powder is reduced with para-aminophenol | |
| CN106694904A (en) | Preparation method of highly dispersed micron order flake silver powder with large radius-thickness ratio | |
| CN104341860A (en) | Nanometer conductive ink and preparing method thereof | |
| CN102220045A (en) | Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof | |
| CN110586952A (en) | Room temperature preparation method of nano metal powder and conductive ink thereof | |
| CN103737011B (en) | The preparation method of high compaction spherical silver powder | |
| CN101327521B (en) | Wet chemical preparation method containing spherical silver powder | |
| CN106041123B (en) | Hollow silver powder of a kind of positive silver high activity of solar cell and preparation method thereof | |
| CN111496266A (en) | Environment-friendly conductive nano copper ink and preparation method thereof | |
| CN110560702A (en) | method for preparing micron-sized single crystal copper powder at room temperature | |
| CN108080651A (en) | The preparation method of electric slurry nanometer silver-coated copper powder | |
| CN103194117B (en) | Preparation method and application of sintering-free ultrafine silver nanometer printing ink | |
| CN111500121B (en) | Conductive ink for flexible printed electronics and sonochemical synthesis method | |
| KR20050116544A (en) | Method of manufacturing silver powder by chemical reduction | |
| CN104001930B (en) | The preparation method of high-temperature electronic slurry lead/galactic nucleus shell composite powder | |
| CN110756823A (en) | Preparation method of spherical nano silver powder | |
| CN110860700A (en) | Preparation method of flaky nano silver powder | |
| CN106180746B (en) | A kind of preparation method of electrical alloy copper silver powder | |
| CN112371992B (en) | Preparation method of core-shell structure silver powder | |
| CN104227012A (en) | Preparation method for ultra-fine copper powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160224 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |