CN103737011A - Method for preparing high-tap-density spherical silver powder - Google Patents
Method for preparing high-tap-density spherical silver powder Download PDFInfo
- Publication number
- CN103737011A CN103737011A CN201310137872.8A CN201310137872A CN103737011A CN 103737011 A CN103737011 A CN 103737011A CN 201310137872 A CN201310137872 A CN 201310137872A CN 103737011 A CN103737011 A CN 103737011A
- Authority
- CN
- China
- Prior art keywords
- silver powder
- ball shape
- preparation
- jolt ramming
- reducing agent
- 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.)
- Granted
Links
Images
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing high-tap-density spherical silver powder. The method includes the following steps that (1), a silver nitrate solution and a reducing agent are respectively prepared, and the temperature of the silver nitrate solution and the temperature of the reducing agent are respectively lowered to range from 0 DEGC to 20 DEG C, wherein the concentration of the silver nitrate solution ranges from 1g/L to 50g/L, and the concentration of the reducing agent ranges from 1g/L to 250g/L; (2), a polymer protective agent and a complexing agent are added into the silver nitrate solution, and the polymer protective agent, the complexing agent and the silver nitrate solution are evenly mixed; (3), under the stirring condition, the reducing agent is added into the silver nitrate solution obtained in the second step; (4), the solution obtained in the third step is continuously stirred till the color of the solution does not change any more and is subjected to centrifugal separation or free settling, and the solution is washed by deionized water several times and is then washed by absolute ethyl alcohol several times; (5), vacuum drying is carried out under the temperature ranging from 50 DEG C to 80 DEG C, and then the high-tap-density spherical silver powder with the grain size ranging from 1 micrometer to 3 micrometers is obtained. Mass production can be achieved by adopting the method for preparing the high-tap-density spherical silver powder, and the prepared high-tap-density spherical silver powder has the ultra-small grain size ranging within the narrow range from 1 micrometer to 3 micrometers and has a high degree of sphericity and smooth surfaces.
Description
Technical field
The present invention relates to a kind of preparation method of silver powder, relate in particular to a kind of preparation method of high jolt ramming ball shape 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, with powder (especially silver powder), prepare various conductive pastes and thick film ink, be widely used in the coating and circuit interconnection of printed circuit.The features such as the development rapidly of photovoltaic industry, has higher requirement to silver powder especially in recent years, and it is large that it requires silver powder to have tap density, good dispersion.Preparing at present silver powder both at home and abroad has a lot of methods, as thermal decomposition method, electrochemical process, aeroponics, wet chemistry method etc.Wherein to have production technology simple for wet chemistry method, the advantage such as particle diameter is controlled and enjoy attention.At wet chemistry method, prepare in ball shape silver powder, generally all with AgNO3, Ag2CO3, [Ag (NH3) 2]
+and silver other compounds as silver-colored source, reducing agent also has a lot, as formaldehyde, formates, hydrazine hydrate, glucose, polyalcohol, ferrous salt, ascorbic acid etc.In order to control reaction speed, realize control silver powder particle diameter, a lot of people have done a lot of work, and the patent that is CN1106326A as publication number adopts alkanolamine to serve as complexing agent, under PH cushioning liquid exists, temperature, in the time of 10-100 ℃, is reacted, and generates dense packing, spherical shaped spherical powder particle.But the method reagent dosage is 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 the protective agent as galactic nucleus growth course such as polyvinylpyrrolidone (PVP), alkyl hydrosulfide (RSH), ammoniacal liquor serves as complexing agent, and Vc is as reducing agent.This patent is that silver nitrate is made into silver ammino solution as silver-colored source, then adds reducing agent to prepare silver powder.Although the silver powder making has the advantages such as stability, good dispersion, is not suitable for suitability for industrialized production.Publication number is that the patent of CN1387968A adopts carbonate to serve as complexing agent, surfactant is that protective agent is prepared 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 jolt ramming ball shape silver powder, the method can not only realize batch production, and the silver powder of preparing is that particle diameter is ultra-fine, in the very narrow scope of 1-3 μ m, distribute, and there is good sphericity and comparatively smooth surface.
The present invention for the technical scheme that solves its technical problem and adopt is: a kind of preparation method of high jolt ramming ball shape silver powder, comprises the following steps:
1. prepare respectively liquor argenti nitratis ophthalmicus and reductant solution, liquor argenti nitratis ophthalmicus concentration is 1-50g/L, and reductant solution concentration is at 1-250g/L, and liquor argenti nitratis ophthalmicus and reductant solution are all cooled to 0-20 ℃;
2. in described liquor argenti nitratis ophthalmicus, add macromolecule dispersant and complexing agent, mix;
3. under stirring condition, by the disposable described reducing agent step that joins 3. in gained liquor argenti nitratis ophthalmicus;
4. above-mentioned solution is constantly stirred, until solution colour no longer changes, then after centrifugation or natural subsidence, first with deionized water washing for several times, then with absolute ethanol washing for several times;
5. vacuum drying under 50-80 ℃ of condition, obtains the high jolt ramming ball shape silver powder of particle diameter in 1-3 μ m 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 adjacent this dicarboxylic acid anhydride 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, the above organic acid of binary or binary or acid anhydrides are complexing agent; 2. there is technique simple, easy to operate, reproducible, non-environmental-pollution advantage; 3. can be according to different customer requirements, produce 1-3 μ m different-grain diameter and obtain spherical powder; 4. the ball shape silver powder produced has the feature of good sphericity and comparatively smooth surface, good dispersion, purity high (>=99.5%), the ideal material of producing various thick-film electronic slips, electronics adhesive, as anisotropic conducting resinl/film.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 1;
Fig. 2 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 2;
Fig. 3 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 3;
Fig. 4 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 4;
Fig. 5 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 5;
Fig. 6 is the shape appearance figure of silver powder SEM × 1000 that make of the embodiment of the present invention 6;
The specific embodiment
By reference to the accompanying drawings, the present invention is elaborated, but protection scope of the present invention is not limited to following embodiment, the simple equivalence of in every case being done with the present patent application the scope of the claims and description changes and modifies, within all still belonging to 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 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 50 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 1, has the better sphericity that obtains, and average grain diameter is 1.5 μ m, good dispersion, and particle diameter narrow distribution, 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 again 5gVc deionized water dissolving constant volume in 50ml (100g/L).Both are all cooled to 8 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 65 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 2, has the better sphericity that obtains, and average grain diameter is 3.0 μ m, good dispersion, and 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 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 50 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 3, has the better sphericity that obtains, and average grain diameter is 1.0 μ m, good dispersion, and particle diameter narrow distribution, 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 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 60 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 4, has the better sphericity that obtains, and average grain diameter is 2.0 μ m, good dispersion, and particle diameter narrow distribution, 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 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 70 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 5, has the better sphericity that obtains, and average grain diameter is 2.7 μ m, good dispersion, and particle diameter narrow distribution, 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 ℃.Then under stirring condition, both are mixed as early as possible completely.Until solution colour no longer changes.Centrifugation, with deionized water washing 3 times, then uses absolute ethanol washing 2 times, and at 80 ℃, vacuum drying obtains silver powder.Gained silver powder as shown in Figure 6, has the better sphericity that obtains, and average grain diameter is 3.0 μ m, good dispersion, and particle diameter narrow distribution, purity is high, tap density 4.3g/cm
3.
Claims (7)
1. a preparation method for high jolt ramming ball shape silver powder, is characterized in that comprising the following steps:
1. prepare respectively liquor argenti nitratis ophthalmicus and reductant solution, liquor argenti nitratis ophthalmicus concentration is 1-50g/L, and reductant solution concentration is at 1-250g/L, and liquor argenti nitratis ophthalmicus and reductant solution are all cooled to 0-20 ℃;
2. in described liquor argenti nitratis ophthalmicus, add macromolecule dispersant and complexing agent, mix;
3. under stirring condition, by the disposable described reducing agent step that joins 3. in gained liquor argenti nitratis ophthalmicus;
4. above-mentioned solution is constantly stirred, until solution colour no longer changes, then after centrifugation or natural subsidence, first with deionized water washing for several times, then with absolute ethanol washing for several times;
5. vacuum drying under 50-80 ℃ of condition, obtains the high jolt ramming ball shape silver powder of particle diameter in 1-3 μ m scope.
2. the preparation method of high jolt ramming ball shape 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 jolt ramming ball shape 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 jolt ramming ball shape silver powder according to claim 1, is characterized in that: described complexing agent be with the organic acid of two carboxyls and plural carboxyl or acid anhydrides one of them.
5. the preparation method of high jolt ramming ball shape silver powder according to claim 4, is characterized in that: described complexing agent be phthalic acid and adjacent this dicarboxylic acid anhydride one of them.
6. the preparation method of high jolt ramming ball shape 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.
7. the preparation method of high jolt ramming ball shape 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 true CN103737011A (en) | 2014-04-23 |
| CN103737011B 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) |
Cited By (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 (6)
| 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 |
| JP2009235474A (en) * | 2008-03-26 | 2009-10-15 | Dowa Electronics Materials Co Ltd | Method for producing 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 |
-
2013
- 2013-04-22 CN CN201310137872.8A patent/CN103737011B/en not_active Expired - Fee Related
Patent Citations (6)
| 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 |
| JP2009235474A (en) * | 2008-03-26 | 2009-10-15 | Dowa Electronics Materials Co Ltd | Method for producing silver powder |
| 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 |
|---|
| 宋永辉等: "球形纳米银粉的制备研究", 《稀有金属材料与工程》 * |
| 敖毅伟等: "化学还原法中制备条件对超细银粉形貌的影响", 《粉末冶金技术》 * |
Cited By (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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103737011B (en) | 2016-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7648557B2 (en) | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom | |
| US8372178B2 (en) | Silver particles and processes for making them | |
| US8366799B2 (en) | Silver particles and a process for making them | |
| US20100279116A1 (en) | Silver particles and processes for making them | |
| CN102407341B (en) | surface modified particle diameter mixed silver powder and preparation method thereof | |
| CN104096850B (en) | The method that silver ammonia complex prepares superfine spherical silver powder is reduced with para-aminophenol | |
| CN102343441A (en) | Method for preparing monodispersed silver powder with high tap density and low agglomeration | |
| CN104845449A (en) | Preparation and application of RFID antenna-based inkjet conductive ink | |
| CN110586952A (en) | Room temperature preparation method of nano metal powder and conductive ink thereof | |
| CN107685156A (en) | The preparation method of silver nanocubes | |
| CN103737011B (en) | The preparation method of high compaction spherical silver powder | |
| CN101327521B (en) | Wet chemical preparation method containing spherical silver powder | |
| CN111496266A (en) | Environment-friendly conductive nano copper ink and preparation method thereof | |
| CN107759464B (en) | Controllable preparation method of monodisperse copper oxalate powder | |
| CN106513706B (en) | A kind of preparation method for being used for Nano Silver nucleus in ball shape silver powder production technology | |
| KR100631025B1 (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 | |
| CN108080651A (en) | The preparation method of electric slurry nanometer silver-coated copper powder | |
| CN106519302A (en) | Laser-forming plastic active additive and preparation method thereof | |
| CN110860700A (en) | Preparation method of flaky nano silver powder | |
| KR100368055B1 (en) | Synthesis of Spherical Fine Silver Powders at Room Temperature | |
| CN110756823A (en) | Preparation method of spherical nano silver powder | |
| CN105679408B (en) | The acrylic acid microcapsules processing method of copper powder in a kind of electric slurry | |
| CN112091233B (en) | Synthesis method of silver nanoparticles | |
| 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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160224 |