CN102114546A - Method for preparing spherical silver powder - Google Patents
Method for preparing spherical silver powder Download PDFInfo
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- CN102114546A CN102114546A CN 201110076231 CN201110076231A CN102114546A CN 102114546 A CN102114546 A CN 102114546A CN 201110076231 CN201110076231 CN 201110076231 CN 201110076231 A CN201110076231 A CN 201110076231A CN 102114546 A CN102114546 A CN 102114546A
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Abstract
The invention discloses a method for preparing spherical silver powder, relating to a method for preparing conductive silver paste in electronic industry. The method for preparing spherical silver powder is characterized by comprising the following steps: atomizing the dissolvable silver salt solution, carrying out thermal decomposition under conditions of high temperature and controllable atmosphere and then preparing spherical silver powder. In the method, the dissolvable silver salt solution is used as raw materials and is atomized, and then thermal decomposition is conducted to the mixing solution at high temperature and under controllable atmosphere so as to generate the spherical silver powder. With the method, the preparation process from the solution to the spherical silver powder can be continuously realized by one step, the granularity of the prepared spherical silver powder is controllable within the range of 0.2-20 micrometers, the granularity of the powder is uniformly distributed and has even compositions and is excellent in performance. The preparation method is energy-saving and environment-friendly, and has low production cost and obvious economic and social benefits.
Description
Technical field
A kind of preparation method of ball shape silver powder relates to and is used for the preparation method that the electronics industry conductive silver is starched the ball shape silver powder of preparation.
Background technology
Ball shape silver powder is mainly used in manufacturing conductive silver slurry in the electronics industry, comprises that the internal and external electrode silver that slice component is used is starched, thick film integrated circuit conductor silver is starched, Taihang can be starched or the like by battery electrode silver.
The conductive silver slurry is meant and is printed on the conduction stock, makes it to have the silver slurry of conductive capability, generally is to be imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard.The silver slurry that the photovoltaic industry is used is printed on solar cell surface, uses as electrode.The quality of the situation that the silver slurry prints electrode on cell panel, silver slurry directly has influence on the photoelectric transformation efficiency of battery, and it is realized by top layer Metal Contact device typography efficient the influence of efficient.The critical material of silver slurry usefulness is a silver powder, and this silver slurry is very high to the requirement of silver powder, as aspects such as dispersiveness, tap density, electric conductivity.
At present, the internal and external electrode of China's slice component (chip inductor, sheet capacitor, plate resistor) usefulness silver slurry needs import more than 80%; And the silver of some specific use aspect slurry, as thick film integrated circuit conductor silver slurry, Taihang can battery electrode silver slurry, the automobile back windshield defrost with silver is starched, conductive adhesive is used silver conductive adhesive, electromagnetic shielding with silver-colored electrically-conducting paint etc., 90% above dependence on import then, electrode of solar battery conductor silver slurry all needs import to solve especially.It is predicted that China's solar cell yield will reach 25GW in 2011, need the silver slurry to reach 4000 tons, promptly need 3200 tons in silver powder.The silver paste of solar cells of China's development still belongs to blank with silver powder, can not adapt to the needs of China's manufacture of solar cells high speed development far away, has become the bottleneck of restriction China solar cell development.
Liquid phase reduction is the topmost method of preparation silver powder at present.It is soluble in water to be about to silver salt (silver nitrate etc.), add chemical reducing agent (as hydrazine hydrate etc.), deposit silver powder, obtain silver-colored reduced powder through washing, drying, particle diameter is between 0.2-20 μ m, the use of the selection of reducing agent, the control of reaction condition, interfacial agent can prepare the micro silver powder of different physicochemical characteristics.But exist long flow path, batch between difference big, cost is high and problem such as seriously polluted; Also has atomization in addition, promptly with the silver atomizing of medium with fusion, thereby formation ball shape silver powder, atomization is simple to operate, product purity is high, crystal property is good, but be subjected to the restriction of its equipment, but problems such as the silver powder that this method is produced exists size distribution inhomogeneous, and particle is excessive can't be produced high-quality ball shape silver powder.
The high temperature pyrolysis flouring technology is the advanced problem of domestic and international powder production field.At present, adopt spray pyrolysis preparation of industrialization powder body material, the application that particularly prepares the silver powder aspect yet there are no report.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, and a kind of preparation method with advantage such as technological process is short, cost is low, environmental protection and energy saving and ball shape silver powder that product is even, purity is high, electric conductivity is high is provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of ball shape silver powder is characterized in that its preparation process with after the liquor argenti nitratis ophthalmicus atomizing, at high temperature carries out thermal decomposition and directly produce ball shape silver powder.
The preparation method of a kind of ball shape silver powder of the present invention is characterized in that described silver salt solution is a liquor argenti nitratis ophthalmicus.
The preparation method of a kind of ball shape silver powder of the present invention is characterized in that the argent ion concentration in the described liquor argenti nitratis ophthalmicus is 10～400g/L.
The preparation method of a kind of ball shape silver powder of the present invention is characterized in that described liquor argenti nitratis ophthalmicus atomizing is the drop of 0.5～100 μ m.
The preparation method of a kind of ball shape silver powder of the present invention is characterized in that drop after the atomizing of described liquor argenti nitratis ophthalmicus under 200～900 ℃ of temperature, thermal decomposition 1～30 minute.
The preparation method of a kind of ball shape silver powder of the present invention is characterized in that described controlled atmosphere condition is a kind of in nitrogen, hydrogen, the carbon monoxide.
The preparation method of a kind of ball shape silver powder of the present invention, as raw material, the atomizing back makes the silver nitrate pyrolysis generate ball shape silver powder in high temperature (200～900 ℃), controlled atmosphere with liquor argenti nitratis ophthalmicus, produces tail gas through absorbing the method that forms regenerated acid.This method can realize the preparation process from solution to the ball shape silver powder step continuously, and the ball shape silver powder powder size that this method makes is controlled in 0.2～20 micrometer range, and powder size is evenly distributed, the electric conductivity height.These preparation method's energy-saving and environmental protection, production cost are low, have remarkable economical and social benefit.
Description of drawings
Fig. 1 is the stereoscan photograph of the prepared ball shape silver powder of the present invention.
Fig. 2 is the process chart of method of the present invention.
The specific embodiment
A kind of preparation method of ball shape silver powder powder body material, its preparation process are with after the liquor argenti nitratis ophthalmicus atomizing, at high temperature carry out thermal decomposition and obtain the ball shape silver powder powder body material.The step of preparation process comprises:
1) batching: liquor argenti nitratis ophthalmicus is the preparation of 10～400g/L concentration by concentration of silver ions.
2) solution atomization is the drop of 0.5～100 μ m atomizing: will prepare burden 1).
3) pyrolysis: with 2) the gained drop is under 200～900 ℃, controlled atmosphere condition (nitrogen, hydrogen, carbon monoxide), pyrolysis 1～30 minute.
Embodiment 1
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 100g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 300 ℃, hydrogen reducing atmosphere condition, heat 30min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 1 μ m, tap density is 1.42g/cm
3, oxygen content 0.1%.
Embodiment 2
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 100g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 500 ℃, carbon monoxide reducing atmosphere condition, heat 10min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 2 μ m, tap density is 2.45g/cm
3
Embodiment 3
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 100g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 700 ℃, nitrogen protection atmospheric condition, heat 10min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 3.2 μ m, tap density is 3.54g/cm
3
Embodiment 4
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 100g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 900 ℃, nitrogen protection atmospheric condition, heat 10min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 4 μ m, tap density is 4.75g/cm
3
Embodiment 5
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 10g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 400 ℃, carbon monoxide reducing atmosphere condition, heat 30min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 1 μ m, tap density is 2.21g/cm
3
Embodiment 6
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 300g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 700 ℃, hydrogen reducing atmosphere condition, heat 10min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 3.8 μ m, tap density is 4.06g/cm
3
Embodiment 7
The configuration concentration of silver ions is the liquor argenti nitratis ophthalmicus of 400g/L; Solution is atomized through atomizer; The drop of atomizing is sprayed in the heating furnace, under temperature is 800 ℃, hydrogen reducing atmosphere condition, heat 5min.Gained ball shape silver powder complete in crystal formation, no dephasign, even particle size distribution, D50 is 4.4 μ m, tap density is 4.83g/cm
3
Technological process of the present invention is simple and direct, and decomposition atmosphere is controlled, the capacity usage ratio height, and impurity content is low, can significantly improve the powder agglomeration traits, the product quality excellence.The chemical waste fluid discharging of nonpollution environment.Tail gas can be absorbed purification, and emission gases reaches national environmental standard.
Claims (6)
1. the preparation method of a ball shape silver powder, it is characterized in that its preparation process is with the liquor argenti nitratis ophthalmicus atomizing after, under high temperature controlled atmosphere condition, carry out thermal decomposition and directly produce ball shape silver powder.
2. the preparation method of a kind of ball shape silver powder according to claim 1 is characterized in that used silver salt solution is a liquor argenti nitratis ophthalmicus.
3. the preparation method of a kind of ball shape silver powder according to claim 1 is characterized in that the argent ion concentration in the described silver salt solution is 10～400g/L.
4. a kind of ball shape silver powder powder body material preparation method according to claim 1 is characterized in that described silver salt solution atomizing is the drop of 0.5～100 μ m.
5. a kind of ball shape silver powder powder body material preparation method according to claim 1 is characterized in that drop after the atomizing of described silver salt solution under 200～900 ℃ of temperature, thermal decomposition 1～30 minute.
6. a kind of ball shape silver powder powder body material preparation method according to claim 1 is characterized in that described controlled atmosphere condition is a kind of in nitrogen, hydrogen, the carbon monoxide.
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| CN 201110076231 CN102114546A (en) | 2011-03-29 | 2011-03-29 | Method for preparing spherical silver powder |
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| CN 201110076231 CN102114546A (en) | 2011-03-29 | 2011-03-29 | Method for preparing spherical silver powder |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528075A (en) * | 2012-03-15 | 2012-07-04 | 中南大学 | Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate |
| CN103143725A (en) * | 2013-03-29 | 2013-06-12 | 赣州远驰新材料有限公司 | Method for preparing rare earth modified tungsten-base alloy powder |
| CN103317148A (en) * | 2013-06-07 | 2013-09-25 | 惠州市富济电子材料有限公司 | Silver powder and silver colloid prepared with silver powder |
| CN103350233A (en) * | 2013-06-29 | 2013-10-16 | 西北矿冶研究院 | Spray pyrolysis method silver powder production system and production method thereof |
| CN104174858A (en) * | 2013-05-27 | 2014-12-03 | 刘建 | Preparation method of silver powder or doped silver powder |
| CN105263656A (en) * | 2013-05-24 | 2016-01-20 | 田中贵金属工业株式会社 | Method for producing silver particles |
| CN103962569B (en) * | 2013-01-30 | 2016-08-17 | 比亚迪股份有限公司 | A kind of preparation method of flake silver powder |
| CN116072350A (en) * | 2023-04-07 | 2023-05-05 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2080052T3 (en) * | 1988-04-16 | 1996-02-01 | Duerrwaechter E Dr Doduco | POWDER METALLURGICAL PROCEDURE FOR THE PRODUCTION OF A SEMI-TERMINATED PART FOR ELECTRICAL CONTACTS MADE OF A SILVER BASED COMPOSITE MATERIAL, WITH IRON. |
| CN1557163A (en) * | 2004-02-13 | 2004-12-29 | 黄德欢 | Nano antiseptic silver powder preparation method using metallic silver |
| CN101214555A (en) * | 2008-01-16 | 2008-07-09 | 武汉理工大学 | Method for preparing spherical nano silver powder |
| CN101885072A (en) * | 2010-07-01 | 2010-11-17 | 苏州永拓环境科技有限公司 | Preparation method of nano-silver sol |
-
2011
- 2011-03-29 CN CN 201110076231 patent/CN102114546A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2080052T3 (en) * | 1988-04-16 | 1996-02-01 | Duerrwaechter E Dr Doduco | POWDER METALLURGICAL PROCEDURE FOR THE PRODUCTION OF A SEMI-TERMINATED PART FOR ELECTRICAL CONTACTS MADE OF A SILVER BASED COMPOSITE MATERIAL, WITH IRON. |
| CN1557163A (en) * | 2004-02-13 | 2004-12-29 | 黄德欢 | Nano antiseptic silver powder preparation method using metallic silver |
| CN101214555A (en) * | 2008-01-16 | 2008-07-09 | 武汉理工大学 | Method for preparing spherical nano silver powder |
| CN101885072A (en) * | 2010-07-01 | 2010-11-17 | 苏州永拓环境科技有限公司 | Preparation method of nano-silver sol |
Non-Patent Citations (1)
| Title |
|---|
| 《中国有色金属学报》 20070131 刘志宏 等 "喷雾热分解法制备超细银粉及其形貌控制" 第149-155页 1 第17卷, 第1期 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528075A (en) * | 2012-03-15 | 2012-07-04 | 中南大学 | Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate |
| CN102528075B (en) * | 2012-03-15 | 2013-12-18 | 中南大学 | Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate |
| CN103962569B (en) * | 2013-01-30 | 2016-08-17 | 比亚迪股份有限公司 | A kind of preparation method of flake silver powder |
| CN103143725A (en) * | 2013-03-29 | 2013-06-12 | 赣州远驰新材料有限公司 | Method for preparing rare earth modified tungsten-base alloy powder |
| CN103143725B (en) * | 2013-03-29 | 2015-08-12 | 赣州远驰新材料有限公司 | The preparation method of rare earth modified tungsten-base alloy powder |
| CN105263656A (en) * | 2013-05-24 | 2016-01-20 | 田中贵金属工业株式会社 | Method for producing silver particles |
| CN104174858A (en) * | 2013-05-27 | 2014-12-03 | 刘建 | Preparation method of silver powder or doped silver powder |
| CN103317148A (en) * | 2013-06-07 | 2013-09-25 | 惠州市富济电子材料有限公司 | Silver powder and silver colloid prepared with silver powder |
| CN103317148B (en) * | 2013-06-07 | 2015-11-25 | 惠州市富济电子材料有限公司 | A kind of silver powder and gained elargol |
| CN103350233A (en) * | 2013-06-29 | 2013-10-16 | 西北矿冶研究院 | Spray pyrolysis method silver powder production system and production method thereof |
| CN103350233B (en) * | 2013-06-29 | 2016-07-06 | 西北矿冶研究院 | Method for producing silver powder by spray pyrolysis method |
| CN116072350A (en) * | 2023-04-07 | 2023-05-05 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
| CN116072350B (en) * | 2023-04-07 | 2023-08-15 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
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Application publication date: 20110706 |