CN105583407A - Preparation method of single-dispersion and high-tap-density spherical silver powder - Google Patents
Preparation method of single-dispersion and high-tap-density spherical silver powder Download PDFInfo
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Abstract
The invention provides a preparation method of single-dispersion and high-tap-density spherical silver powder. Silver nitrate is selected as a raw material, ascorbic acid is selected as a reducing agent, and a certain quantity of organic dispersing agent A is added to prepare high-dispersed spherical silver powder by a chemical codeposition method; the particle size distribution tested by a laser particle size analyzer is substantially corresponding to the particle size of once silver particles in a scanning electron microscope picture; meanwhile, the particle size of the silver powder is controllable; the average particle size is 0.69-2.53 microns; the specific surface area is 0.82-1.84 m2/g; and the tap density is 5.1-7.6 g/cm3. The silver powder can be applied to preparation of high-level silver conductor slurry; and the prepared silver slurry has such advantages as high electric conductivity and high resolution.
Description
Technical field
The present invention relates to the preparation method of ball shape silver powder, particularly relate to monodispersity, high-tap density,The preparation method of the ball shape silver powder of low specific surface area.
Background technology
Along with the development of electronic information technology, chip components and parts and integrated circuit will have more wide market,This also brings opportunity to develop to the application prospect of electric slurry. Noble metal conductor paste is to make in integrated circuitWith maximum a kind of materials, occupy main material cost, the quality of noble metal conductor paste is designOne of principal element of considering when integrated circuit. Noble metal conductor paste is a lot, different occupation mode,Attaching substrates, electricity, mechanical performance requirement, all by producing different noble metal conductor pastes, from applicationIn temperature, can be divided into low temperature curing type and high temperature sintering type, but say from basic composition, be all byConducting function phase, bonding phase and organic carrier three part compositions. In numerous noble metal conductor pastes,Silver slurry occupies most ratios, and the performance of silver conductive paste is mainly determined by silver powder, the pattern of silver powder,The parameters such as particle diameter distribution, apparent density, tap density, specific area, degree of scatter directly affect silver and leadThe performance of somaplasm material.
In recent years, because solar energy industry is in fast development, make domestic for solar battery front side electricityExtremely the demand of silver slurry sharply increases, this front side silver paste demand be exactly a kind of high degree of dispersion, high vibration densityThe ball shape silver powder of degree, makes front side silver paste in Fast Sintering process, and in silver layer, defect is few, and density is high,Possess good electric conductivity, be conducive to improve the electricity conversion of solar cell. In addition, for oneThe silver slurry of the sintering that need to (be greater than 800 DEG C) under higher temperatures condition a bit, such as electrode silver in multilayer co-firingSlurry, table back electrode that slice component is used silver slurry etc., sintering temperature all 850 DEG C and more than, adopt Gao ZhenThe monodispersed ball shape silver powder of real density, is conducive to improve resistance to sintering temperature, the silver-colored palladium slurry of an alternative part,Significantly reduce costs.
Summary of the invention
Content of the present invention is to adopt chemical codeposition legal system for silver powder, by control oxygen in course of reactionThe concentration of agent and reducing agent, the type of dispersant and consumption, solution drip mode, pH value, stirring speedThe parameters such as degree, develop single ball shape silver powder that disperses high-tap density.
For achieving the above object, the invention provides following technical scheme: a kind of single high vibration density of disperseingThe preparation method of degree ball shape silver powder, described single high tap density spherical silver powder that disperses is by chemical codeposition legal systemStandby; It is characterized in that, it is silver material that described chemical codeposition method adopts silver nitrate, and ascorbic acid is reductionAgent, adds dispersant A, and under the condition that adds thermal agitation, reaction generates silver powder.
As improvement, described chemical codeposition method comprises the steps:
(1) take 50-102 gram of silver nitrate and be dissolved in 1L deionized water, stir, dissolve, be mixed with nitreThe silver-colored solution of acid;
(2) in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and dispersantThe mixed solution of A;
(3) taking the ascorbic acid of 40-80 gram is dissolved in 500ml deionized water and is mixed with reducing solution;
(4) mixed solution of silver nitrate and dispersant A and reducing solution are stirred 25-30 DEG C of water bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, by the mixed solution of silver nitrate and dispersant ASlowly pour in ascorbic acid solution reducing solution and stir, mixing speed is 200-350rpm, then by nitreThe silver-colored solution of acid drops in mixed solution, and rate of addition is 20-250ml/s, after dripping, continues to stirAfter reaction 3-10min, obtain flaxen suspension.
(5) silver-colored suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateThe silver powder getting off is successively with deionized water washing 3-10 time;
(6) then taking organic matter B is dissolved in its 5 times of absolute ethyl alcohols, by the ethanolic solution of organic matter BBe poured in washed silver slurry, stir;
(7) in drying box in 50-70 DEG C, after dry 8-30h, adopt the sides such as machinery or air-flow crushingFormula is beaten powder.
Described dispersant A be polyvinyl alcohol, succinic acid, polyvinylpyrrolidone, gelatin, polyethylene glycol,The mixture of one or more in carboxymethyl cellulose. The mass ratio of dispersant A and AgNO3 is1-40: 100. Further improve, the mass ratio of dispersant A and AgNO3 is 5-20: 100. Described haveMachine thing B is the one in glyceryl monostearate, APEO fatty alcohol, Arabic gum, stearic acidOr more than one mixture. Concentration at liquor argenti nitratis ophthalmicus described in step (1) is 0.2-0.6mol/L,The concentration of ascorbic acid is 0.45-0.9mol/L.
Finally, single average grain diameter of disperseing high tap density spherical silver powder that the method is prepared is0.69-2.53 μ m, specific area is 0.82-1.84m2/g, tap density is 5.1-7.6g/cm3.
Compared with prior art, the invention has the beneficial effects as follows: than the silver powder of current common use,The tap density of this silver powder exceeds 2~4 times, and monodispersity can be good, and oil absorption is little; The high jolt ramming of this single dispersionThe successful development of density ball shape silver powder, large-scale production, the kind that can expand silver powder, for some are high-endThe research and production of silver conductive paste provides materials for support; Utilize silver slurry prepared by this silver powder to possess high temperature resistantThe advantages such as sintering, electrical conductivity is high, the few loss of defect is little, dispersive property good, linear resolution is high.
Brief description of the drawings
Fig. 1 is process chart of the present invention.
Fig. 2 is the SEM figure that the embodiment of the present invention is prepared the mono-dispersion of 1# high tap density spherical silver powder.
Fig. 3 is the SEM figure that the embodiment of the present invention is prepared the mono-dispersion of 2# high tap density spherical silver powder.
Fig. 4 is the SEM figure that the embodiment of the present invention is prepared the mono-dispersion of 3# high tap density spherical silver powder.
Fig. 5 is the SEM figure that the embodiment of the present invention is prepared the mono-dispersion of 4# high tap density spherical silver powder.
Fig. 6 is the laser particle analyzer survey that the embodiment of the present invention is prepared the mono-dispersion of 1# high tap density spherical silver powderTest result.
Fig. 7 is the laser particle analyzer survey that the embodiment of the present invention is prepared the mono-dispersion of 2# high tap density spherical silver powderTest result.
Fig. 8 is the laser particle analyzer survey that the embodiment of the present invention is prepared the mono-dispersion of 3# high tap density spherical silver powderTest result.
Fig. 9 is the laser particle analyzer survey that the embodiment of the present invention is prepared the mono-dispersion of 4# high tap density spherical silver powderTest result.
Detailed description of the invention
The selection of solution and preparation:
Dispersant A is polyvinyl alcohol, succinic acid, polyvinylpyrrolidone, gelatin, polyethylene glycol, carboxylic firstOne or more mixtures in base cellulose;
Organic matter B is in glyceryl monostearate, APEO fatty alcohol, Arabic gum, stearic acidOne or more mixture; Organic matter B is dissolved in self absolute ethyl alcohol of 5 times.
Embodiment mono-:
The silver nitrate that takes 50 grams is dissolved in 1L deionized water, stirs it is fully dissolved, and is mixed with nitric acidSilver solution; Then in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and divideThe mixed solution of powder A; Wherein, the mass ratio of dispersant A and silver nitrate is 0.4: 1; Next take40 grams of ascorbic acid are dissolved in and in 500ml deionized water, are mixed with ascorbic acid reducing solution.
The mixed solution of silver nitrate and dispersant A and ascorbic acid reducing solution are stirred 30 DEG C of waters bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, the mixed solution of silver nitrate and dispersant A is slowSlow pouring in ascorbic acid solution reducing solution also stirred, and mixing speed is 200rpm, and rate of addition is20ml/s, after dripping, continues to obtain flaxen suspension after stirring reaction 5min.
Silver suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateSilver powder successively with deionized water washing 7 times;
Then take 0.6g organic matter B and be dissolved in 3g absolute ethyl alcohol, the ethanolic solution of organic matter B is poured intoIn washed silver slurry, stir.
Finally in drying box after 60 DEG C of dry 8h, adopt the modes such as machinery or air-flow crushing to beat powder,Obtain the monodispersed super fine silver powder of 1#, as shown in Table 1, ESEM picture, as Fig. 2, swashs design parameterThe particle diameter distribution map of light Particle Size Analyzer test as shown in Figure 6.
Embodiment bis-:
The silver nitrate that takes 50 grams is dissolved in 1L deionized water, stirs it is fully dissolved, and is mixed with nitric acidSilver solution; Then in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and divideThe mixed solution of powder A; Wherein, the mass ratio of dispersant A and silver nitrate is 0.1: 1; Next take40 grams of ascorbic acid are dissolved in and in 500ml deionized water, are mixed with ascorbic acid reducing solution.
The mixed solution of silver nitrate and dispersant A and ascorbic acid reducing solution are stirred 30 DEG C of waters bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, the mixed solution of silver nitrate and dispersant A is slowSlow pouring in ascorbic acid solution reducing solution also stirred, and mixing speed is 200rpm, and rate of addition is20ml/s, after dripping, continues to obtain flaxen suspension after stirring reaction 5min.
Silver suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateSilver powder successively with deionized water washing 5 times;
Then take 0.4g organic matter B and be dissolved in 2g absolute ethyl alcohol, the ethanolic solution of organic matter B is poured intoIn washed silver slurry, stir.
In final drying case, after 60 DEG C of dry 8h, adopt the modes such as machinery or air-flow crushing to beat powder,Obtain the monodispersed super fine silver powder of 2#, as shown in Table 1, ESEM picture, as Fig. 3, swashs design parameterThe particle diameter distribution map of light Particle Size Analyzer test as shown in Figure 7.
Embodiment tri-:
The silver nitrate that takes 50 grams is dissolved in 1L deionized water, stirs it is fully dissolved, and is mixed with nitric acidSilver solution; Then in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and divideThe mixed solution of powder A; Wherein, the mass ratio of dispersant A and silver nitrate is next to take 40 at 0.1: 1Gram ascorbic acid is dissolved in and in 500ml deionized water, is mixed with ascorbic acid reducing solution.
The mixed solution of silver nitrate and dispersant A and ascorbic acid reducing solution are stirred 30 DEG C of waters bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, the mixed solution of silver nitrate and dispersant A is slowSlow pouring in ascorbic acid solution reducing solution also stirred, and mixing speed is 200rpm, and rate of addition is50ml/s, after dripping, continues to obtain flaxen suspension after stirring reaction 5min.
Silver suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateSilver powder successively with deionized water washing 5 times;
Then take 0.4g organic matter B and be dissolved in 2g absolute ethyl alcohol, the ethanolic solution of organic matter B is poured intoIn washed silver slurry, stir; Wherein, organic matter B is glyceryl monostearate, APEOThe mixture of one or more in fatty alcohol, Arabic gum, stearic acid.
In final drying case, after 60 DEG C of dry 8h, adopt the modes such as machinery or air-flow crushing to beat powder,Obtain the monodispersed super fine silver powder of 2#, as shown in Table 1, ESEM picture, as Fig. 4, swashs design parameterThe particle diameter distribution map of light Particle Size Analyzer test as shown in Figure 8.
Embodiment tetra-:
The silver nitrate that takes 102 grams is dissolved in 1L deionized water, stirs it is fully dissolved, and is mixed with nitric acidSilver solution; Then in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and divideThe mixed solution of powder A; Wherein, the mass ratio of dispersant A and silver nitrate is 0.12: 1; Next take80 grams of ascorbic acid are dissolved in and in 500ml deionized water, are mixed with ascorbic acid reducing solution.
The mixed solution of silver nitrate and dispersant A and ascorbic acid reducing solution are stirred 25 DEG C of waters bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, the mixed solution of silver nitrate and dispersant A is slowSlow pouring in ascorbic acid solution reducing solution also stirred, and mixing speed is 350rpm, and rate of addition is250ml/s, after dripping, continues to obtain flaxen suspension after stirring reaction 5min.
Silver suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateSilver powder successively with deionized water washing 5 times;
Then take 1.5g organic matter B and be dissolved in 7.5g absolute ethyl alcohol, the ethanolic solution of organic matter B is poured intoTo washed silver slurry, stir.
Finally in drying box after 50 DEG C of dry 15h, adopt the modes such as machinery or air-flow crushing to beatPowder, obtains the monodispersed high tap density silver powder of 4#. Design parameter as shown in Table 1, ESEM pictureAs Fig. 5, the particle diameter distribution map of laser particle size analyzer test as shown in Figure 9.
Table 1 prepare 1,2,3, the physical parameter of 4# silver powder sample, comprises that average grain diameter, particle diameter divideCloth (D10, D50 and D90), specific area, apparent density and tap density.
From then in table, can find out: the consumption of described dispersant A affects the pattern of silver powder, particle diameter distributes, comparesSurface area and tap density. Mass ratio as dispersant A and AgNO3 in experiment is 5~20: 100 time, combineClose performance more excellent, the silver powder good sphericity obtaining, monodispersity is good, and tap density is high, narrow diameter distribution,Specific area is little.
Above content is in conjunction with optimum implementation, the present invention to be said the further description of doing, and can not recognizeDetermine specific embodiment of the invention and be only limited to these explanations. It should be appreciated by those skilled in the art, not de-In situation about being limited by appended claims, can carry out in detail various amendments, all should lookFor belonging to protection scope of the present invention.
Claims (8)
1. a single preparation method who disperses high tap density spherical silver powder, described single high-tap density that dispersesBall shape silver powder is standby by chemical codeposition legal system; It is characterized in that, described chemical codeposition method adopts silver nitrateFor silver material, ascorbic acid is reducing agent, adds dispersant A, and under the condition that adds thermal agitation, reaction generatesSilver powder.
2. single preparation method who disperses high tap density spherical silver powder according to claim 1, its spyLevy and be, described chemical codeposition method comprises the steps:
(1) take 50-102 gram of silver nitrate and be dissolved in 1L deionized water, stir, dissolve, be mixed with nitreThe silver-colored solution of acid;
(2) in liquor argenti nitratis ophthalmicus, add dispersant A, stir, dissolve, be mixed with silver nitrate and dispersantThe mixed solution of A;
(3) taking the ascorbic acid of 40-80 gram is dissolved in 500ml deionized water and is mixed with reducing solution;
(4) mixed solution of silver nitrate and dispersant A and reducing solution are stirred 25-30 DEG C of water bath with thermostatic controlMix in device and stir, after treating temperature stabilization half an hour, by the mixed solution of silver nitrate and dispersant ASlowly pour in ascorbic acid solution reducing solution and stir, mixing speed is 200-350rpm, then by nitreThe silver-colored solution of acid drops in mixed solution, and rate of addition is 20-250ml/s, after dripping, continues to stirAfter reaction 3-10min, obtain flaxen suspension.
(5) silver-colored suspension leaves standstill a period of time, then obtains silver powder through sedimentation, Separation of Solid and Liquid, will precipitateThe silver powder getting off is successively with deionized water washing 3-10 time;
(6) then taking organic matter B is dissolved in its 5 times of absolute ethyl alcohols, by the ethanolic solution of organic matter BBe poured in washed silver slurry, stir;
(7) in drying box in 50-70 DEG C, after dry 8-30h, adopt the sides such as machinery or air-flow crushingFormula is beaten powder.
3. single preparation method who disperses high tap density spherical silver powder according to claim 1 and 2,It is characterized in that, described dispersant A be polyvinyl alcohol, succinic acid, polyvinylpyrrolidone, gelatin,The mixture of one or more in polyethylene glycol, carboxymethyl cellulose.
4. single preparation method who disperses high tap density spherical silver powder according to claim 2, its spyLevy and be, the mass ratio of dispersant A and AgNO3 is 1-40: 100.
5. singly disperse according to claim 4 the preparation method of high tap density spherical silver powder, its featureBe, the mass ratio of dispersant A and AgNO3 is 5-20: 100.
6. singly disperse according to claim 2 the preparation method of high tap density spherical silver powder, its featureBe, described organic matter B is glyceryl monostearate, APEO fatty alcohol, Arabic gum, hardThe mixture of one or more in resin acid.
7. singly disperse according to claim 2 the preparation method of high tap density spherical silver powder, its featureBe, the concentration of described liquor argenti nitratis ophthalmicus is 0.2-0.6mol/L, and the concentration of ascorbic acid is0.45-0.9mol/L。
8. according to any single high-tap density ball that disperses described in claim 1,2,4,5,6,7The preparation method of shape silver powder, is characterized in that, single high-tap density spherical silver of disperseing that the method is preparedThe average grain diameter of powder is 0.69-2.53 μ m, and specific area is 0.82-1.84m2/g, and tap density is5.1-7.6g/cm3。
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001107101A (en) * | 1999-10-12 | 2001-04-17 | Mitsui Mining & Smelting Co Ltd | High dispersibility spherical silver powder and its producing method |
CN1709619A (en) * | 2004-06-18 | 2005-12-21 | 同和矿业株式会社 | Spherical silver power and method for producing same |
CN101347841A (en) * | 2008-09-03 | 2009-01-21 | 西北大学 | Method for preparing high tap density silver powder with controllable graininess |
CN101716685A (en) * | 2009-12-14 | 2010-06-02 | 昆明理工大学 | Method for preparing spherical superfine silver powder by using chemical reduction method |
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 |
CN102921944A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Silver powder for printing size for solar cell electrodes and preparation process thereof |
CN103551586A (en) * | 2013-09-22 | 2014-02-05 | 江苏瑞德新能源科技有限公司 | Preparation method of micron spherical silver powder for electroconductive silver paste |
CN103737011A (en) * | 2013-04-22 | 2014-04-23 | 昆山西微美晶电子新材料科技有限公司 | Method for preparing high-tap-density spherical silver powder |
-
2014
- 2014-11-14 CN CN201410690784.5A patent/CN105583407A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001107101A (en) * | 1999-10-12 | 2001-04-17 | Mitsui Mining & Smelting Co Ltd | High dispersibility spherical silver powder and its producing method |
CN1709619A (en) * | 2004-06-18 | 2005-12-21 | 同和矿业株式会社 | Spherical silver power and method for producing same |
CN101347841A (en) * | 2008-09-03 | 2009-01-21 | 西北大学 | Method for preparing high tap density silver powder with controllable graininess |
CN101716685A (en) * | 2009-12-14 | 2010-06-02 | 昆明理工大学 | Method for preparing spherical superfine silver powder by using chemical reduction method |
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 |
CN102921944A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Silver powder for printing size for solar cell electrodes and preparation process thereof |
CN103737011A (en) * | 2013-04-22 | 2014-04-23 | 昆山西微美晶电子新材料科技有限公司 | Method for preparing high-tap-density spherical silver powder |
CN103551586A (en) * | 2013-09-22 | 2014-02-05 | 江苏瑞德新能源科技有限公司 | Preparation method of micron spherical silver powder for electroconductive silver paste |
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