CN102218539A - Method for preparing ultrafine silver powder - Google Patents
Method for preparing ultrafine silver powder Download PDFInfo
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- CN102218539A CN102218539A CN2011101380502A CN201110138050A CN102218539A CN 102218539 A CN102218539 A CN 102218539A CN 2011101380502 A CN2011101380502 A CN 2011101380502A CN 201110138050 A CN201110138050 A CN 201110138050A CN 102218539 A CN102218539 A CN 102218539A
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Abstract
The invention provides a method for preparing ultrafine silver powder, which is characterized in that: an atomization comminuting process is adopted in the method. The silver powder prepared by utilizing the method has the characteristics that the average grain diameter is 0.03-30micrometer, the tap density is more than 3g/cc, the oxygen content is less than 0.05% and the variance of the diameter is less than half of the average diameter. The ultrafine silver powder prepared by utilizing the method provided by the invention has the advantages of low cost, low environmental pollution, low oxygen content and high powder spherical granularity and is suitable for large-scale industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of silver powder, the preparation method of particularly a kind of controllable granularity, highly uniform super fine silver powder.
Background technology
Super fine silver powder is a kind of functional raw material that extensively apply in the electronics industry, as is used for making electric slurry, electrically-conducting paint, electromagnetic screen coating, electrically conductive ink, conductive plastics, conductivity ceramics etc.Its value-added content of product is very high.Yet present problems such as poor, the particle agglomeration of domestic enterprise's silver powder ubiquity uniform granularity of producing, bad dispersibility also do not possess the technology of the super fine silver powder of production high uniformity.High-end silver powder mainly is to rely on external import.For example, the used silver powder of silver paste of solar cells mainly comes from companies such as U.S. DUPANT, FERRO and German Hereaus in the market, has seriously restricted developing of China's related industry.
Present industrial super fine silver powder generally all is to obtain by the liquid phase chemical reduction method.Method as the employing of patents such as CN1700360A, CN1387968A, CN1857833A.Generally be that the solution that will contain reducing agents such as ascorbate joins in the aqueous solution such as liquor argenti nitratis ophthalmicus that contains silver particles, prepare silver powder by reduction reaction.Because Property of Acid and Alkali of Solution is among the variation in the entire reaction course always, therefore the silver powder particles size of preparation is inhomogeneous, broad particle distribution, be more difficult to get be evenly distributed, average grain diameter is at the super fine silver powder below 1 micron.
Summary of the invention:
For the silver powder particle diameter wider distribution that solves the prior art existence, the problem of complex process, the invention provides a kind of preparation method of super fine silver powder, have that low cost, low environment are polluted, the spherical granularity height of powder, oxygen content are low, advantage that can large-scale industrial production.
Technical scheme of the present invention is: a kind of preparation method of super fine silver powder, the gases at high pressure that adopt atomizings or hydraulic atomized method combine with rotating disc centrifugal atomizing method and prepare super fine silver powder, concrete steps are: under vacuum state, liquid galactic longitude nozzle ejection is formed the silvering solution stream that diameter is 1-10mm, working media under high pressure impacts silvering solution stream, the silvering solution that impact grinding forms drips collision on the metal rotating disc of the rotating speed below the nozzle greater than 1000 commentaries on classics/min, carry out the secondary dispersion and fining and obtain silver powder, again through conventional sieving, pickling promptly obtains even-grained, average grain diameter is the 0.03-30 micron, tap density is more than 3g/cc, oxygen content is less than 0.05% super fine silver powder; Described working media is that pressure is that non-reactive gas or the pressure of 1-5MPa is the current of 50-200MPa.
Described non-reactive gas is arbitrary in nitrogen, helium, the argon gas.
Described liquid silver be the fine silver raw material in graphite crucible, vacuum is greater than 10
-2The intensification fusion obtains under the vacuum state of Pa, overheated 100-400 ℃.
Beneficial effect:
(1) the silver powder particle diameter is little, and the average grain diameter of silver powder is the 0.03-30 micron, can prepare the powder of average grain diameter below reaching about 1 micron of the difficult preparation of liquid phase reduction; (2) tap density of silver powder is higher, generally more than 3g/cc; (3) oxygen content of Zhi Bei silver powder is lower than 0.05%; (4) in whole process of preparation, can control the average grain diameter of silver powder by the degree of superheat of regulating metal liquid, diameter, working media and the pressure thereof of metal flow, the parameters such as rotating speed of rotating disc more conveniently; (5) be suitable for suitability for industrialized production, with short production cycle, cost is low, environmental pollution is little.
Description of drawings
Fig. 1 is a preparation facilities schematic diagram of the present invention.
Wherein, 1 is the silvering solution of fusion, and 2 is high-pressure working medium, and 3 is the metal rotating disc.
The specific embodiment
A kind of preparation method of super fine silver powder is the powder by atomization method, to be the rotating disc centrifugal atomizing with gases at high pressure atomizing or hydraulic atomized method the combine preparation of use.
(1) at first the metal fine silver raw material of certain mass is put into graphite crucible, vacuumize.Vacuum is 10
-2More than the Pa;
(2) the argent raw material is heated up melting, overheated 100-400 degree centigrade;
(3) treat silver fusing after, the liquid galactic longitude of high temperature is crossed nozzle and is formed silvering solution stream, the diameter of silvering solution stream is controlled in the 1-10mm scope.
(4) working media under the higher pressure around the nozzle stream of the silvering solution under the impingement flow, liquid silver is fractured into tiny particle rapidly, the working media that adopts can be water or the gas of not giving birth to reaction with silver hair, for example can be nitrogen, helium, argon gas etc., gas pressure is 1-5MPa, and the pressure of current is 50-200MPa.
(5) particle that forms through high-pressure working medium atomizing back collides immediately on the metal rotating disc of rotation at a high speed, carries out the second time and pulverizes and refinement, i.e. rotating disc centrifugal atomizing.Wherein the rotating speed of metal rotating disc is more than 1000 rev/mins.
(6) collect the silver powder of pulverizing through secondary, sieve,, promptly obtain finished product again through conventional surface treatments such as overpicklings.General as required select to vary in size more than 2 kinds greater than 500 purpose screen clothes, remove excessive particle with the bigger screen cloth of mesh earlier, remove too small particle with the less screen cloth of mesh again, just can obtain even-grained target size silver powder.Pickling can be adopted processing such as conventional sulfuric acid, nitric acid.
The preparation method who adopts the gases at high pressure atomizing to combine with the rotating disc centrifugal atomizing.Forvacuum 10
-3Pa is warmed up to 1060 degrees centigrade of fusings with silver, silvering solution flow diameter 4mm, and working media employing purity is 99.95% argon gas, air pressure is 3Mpa, 10000 rev/mins of the rotating speeds of rotating disc.0.05 micron of the silver powder average grain diameter of preparation, tap density 5.6g/cc, oxygen content 0.03%.
Adopt hydraulic atomized preparation method in conjunction with the rotating disc centrifugal atomizing.Forvacuum 10
-3Pa is warmed up to 1180 degrees centigrade of fusings with silver, silvering solution flow diameter 7mm, and working media adopts industrial pure water, and hydraulic pressure is 80Mpa, 12000 rev/mins of the rotating speeds of rotating disc.1.4 microns of the silver powder average grain diameters of preparation, tap density 4.8g/cc, oxygen content 0.04%.
Adopt hydraulic atomized preparation method in conjunction with the rotating disc centrifugal atomizing.Forvacuum 10
-2Pa is warmed up to 1340 degrees centigrade of fusings with silver, silvering solution flow diameter 2mm, and working media adopts industrial pure water, and hydraulic pressure is 150Mpa, 4000 rev/mins of the rotating speeds of rotating disc.18 microns of the silver powder average grain diameters of preparation, tap density 5.9g/cc, oxygen content 0.02%.
Embodiment 4
Adopt the preparation method of gases at high pressure atomizing in conjunction with the rotating disc centrifugal atomizing.Forvacuum 10
-3Pa is warmed up to 1200 degrees centigrade of fusings with silver, silvering solution flow diameter 8mm, and working media employing purity is 99.95% nitrogen, air pressure is 5Mpa, 8000 rev/mins of the rotating speeds of rotating disc.0.35 micron of the silver powder average grain diameter of preparation, tap density 5.1g/cc, oxygen content 0.06%.
Embodiment 5
Adopt the preparation method of gases at high pressure atomizing in conjunction with the rotating disc centrifugal atomizing.Forvacuum 10
-3Pa is warmed up to 1250 degrees centigrade of fusings with silver, silvering solution flow diameter 5mm, and working media employing technical purity is 99.95% argon gas, air pressure is 1Mpa, 2000 rev/mins of the rotating speeds of rotating disc.6.8 microns of the silver powder average grain diameters of preparation, tap density 4.2g/cc, oxygen content 0.018%.
Claims (3)
1. the preparation method of a super fine silver powder, it is characterized in that: the gases at high pressure that adopt atomizings or hydraulic atomized method combine with rotating disc centrifugal atomizing method and prepare super fine silver powder, concrete steps are: under vacuum state, liquid galactic longitude nozzle ejection is formed the silvering solution stream that diameter is 1-10mm, working media under high pressure impacts silvering solution stream, the silvering solution that impact grinding forms drips collision on the metal rotating disc of the rotating speed below the nozzle greater than 1000 commentaries on classics/min, carry out the secondary dispersion and fining and obtain silver powder, again through conventional sieving, pickling promptly obtains even-grained, average grain diameter is the 0.03-30 micron, tap density is more than 3g/cc, oxygen content is less than 0.05% super fine silver powder; Described working media is that pressure is that non-reactive gas or the pressure of 1-5MPa is the current of 50-200MPa.
2. the preparation method of super fine silver powder according to claim 1 is characterized in that: described non-reactive gas is arbitrary in nitrogen, helium, the argon gas.
3. the preparation method of super fine silver powder according to claim 1 is characterized in that: described liquid silver for the fine silver raw material in graphite crucible, vacuum obtains greater than intensification fusion under the vacuum state of 10-2Pa, overheated 100-400 ℃.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103480854A (en) * | 2013-10-09 | 2014-01-01 | 四川有色金源粉冶材料有限公司 | Method for preparing ultrathin metal powder |
| CN103752838A (en) * | 2014-01-23 | 2014-04-30 | 同济大学 | Device for preparing ultra-fine metal powder in multi-stage atomization technique and use method thereof |
| CN104080561A (en) * | 2012-02-02 | 2014-10-01 | 户田工业株式会社 | Silver microparticles, method for producing same, and electronic device, conductive film, and conductive paste containing said silver microparticles |
| CN105583405A (en) * | 2011-11-28 | 2016-05-18 | 重庆有研重冶新材料有限公司 | Method for preparing metal powder in atomizing manner |
| CN106862578A (en) * | 2017-02-13 | 2017-06-20 | 连云港倍特超微粉有限公司 | It is a kind of to combine the apparatus and method that atomization type prepares spherical metal alloy powder |
| CN107282935A (en) * | 2016-12-30 | 2017-10-24 | 西安交通大学青岛研究院 | A kind of continuous liquid supply atomization preparing apparatus of nickel aluminium powder |
| CN107414093A (en) * | 2016-12-30 | 2017-12-01 | 西安交通大学青岛研究院 | A kind of continuous liquid supply atomization preparing apparatus of TiAl powder |
| CN107470644A (en) * | 2016-12-30 | 2017-12-15 | 西安交通大学青岛研究院 | A kind of atomization production of nickel aluminium powder |
| CN110310756A (en) * | 2019-06-28 | 2019-10-08 | 智玻蓝新科技(武汉)有限公司 | A kind of preparation process of the dedicated conductive silver powder of glass base circuit board |
| CN111587056A (en) * | 2020-05-14 | 2020-08-25 | 湖南省国银新材料有限公司 | Electromagnetic shielding silver paste for communication equipment and preparation method thereof |
| CN115570141A (en) * | 2022-12-09 | 2023-01-06 | 长春黄金研究院有限公司 | Preparation method of superfine silver powder for conductive paste |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105583405B (en) * | 2011-11-28 | 2018-04-06 | 重庆有研重冶新材料有限公司 | A kind of method that atomization prepares metal dust |
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| CN104080561A (en) * | 2012-02-02 | 2014-10-01 | 户田工业株式会社 | Silver microparticles, method for producing same, and electronic device, conductive film, and conductive paste containing said silver microparticles |
| CN103480854B (en) * | 2013-10-09 | 2016-05-18 | 四川有色金源粉冶材料有限公司 | A kind of method of preparing submicron metal |
| CN103480854A (en) * | 2013-10-09 | 2014-01-01 | 四川有色金源粉冶材料有限公司 | Method for preparing ultrathin metal powder |
| CN103752838A (en) * | 2014-01-23 | 2014-04-30 | 同济大学 | Device for preparing ultra-fine metal powder in multi-stage atomization technique and use method thereof |
| CN107282935A (en) * | 2016-12-30 | 2017-10-24 | 西安交通大学青岛研究院 | A kind of continuous liquid supply atomization preparing apparatus of nickel aluminium powder |
| CN107414093A (en) * | 2016-12-30 | 2017-12-01 | 西安交通大学青岛研究院 | A kind of continuous liquid supply atomization preparing apparatus of TiAl powder |
| CN107470644A (en) * | 2016-12-30 | 2017-12-15 | 西安交通大学青岛研究院 | A kind of atomization production of nickel aluminium powder |
| CN106862578A (en) * | 2017-02-13 | 2017-06-20 | 连云港倍特超微粉有限公司 | It is a kind of to combine the apparatus and method that atomization type prepares spherical metal alloy powder |
| CN110310756A (en) * | 2019-06-28 | 2019-10-08 | 智玻蓝新科技(武汉)有限公司 | A kind of preparation process of the dedicated conductive silver powder of glass base circuit board |
| CN111587056A (en) * | 2020-05-14 | 2020-08-25 | 湖南省国银新材料有限公司 | Electromagnetic shielding silver paste for communication equipment and preparation method thereof |
| CN115570141A (en) * | 2022-12-09 | 2023-01-06 | 长春黄金研究院有限公司 | Preparation method of superfine silver powder for conductive paste |
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Application publication date: 20111019 |