CN102343441A - Method for preparing monodispersed silver powder with high tap density and low agglomeration - Google Patents
Method for preparing monodispersed silver powder with high tap density and low agglomeration Download PDFInfo
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- CN102343441A CN102343441A CN2011102846641A CN201110284664A CN102343441A CN 102343441 A CN102343441 A CN 102343441A CN 2011102846641 A CN2011102846641 A CN 2011102846641A CN 201110284664 A CN201110284664 A CN 201110284664A CN 102343441 A CN102343441 A CN 102343441A
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Abstract
The invention relates to a method for preparing monodispersed silver powder with high tap density and low agglomeration, and the method is implemented through the following steps of uniformly mixing an acidic silver salt solution with a mixed reducing solution containing a L-ascorbic acid, a protective agent and a surfactant, and stirring the obtained mixture for reaction; and cleaning and then drying the obtained precipitate so as to obtain the monodispersed silver powder with high tap density and low agglomeration. Compared with the prior art, the silver powder prepared by using the method disclosed by the invention is high in tap density, small in particle diameter and dispersive range, high in degree of sphericity of particles, smooth in surface, small in specific surface area and easy for realization of mass production.
Description
Technical field
The present invention relates to the anodal serigraphy of solar cell with silver slurry technical field, especially relate to a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming.
Background technology
It is microminiaturized, integrated, intelligent that microelectronic product is just tending to.In order to adapt to this trend, printed circuit technique is just needing closeer thin and more accurate circuit.For meeting these needs, it is narrower nearer with wire spacing that lead has become.Thereby, to the conductive silver paste that uses in the electronics industry require increasingly high.The silver slurry is a kind of important materials in the electronics industry, and it is formed with certain proportioning modulation by silver powder, resin, organic solvent.The factor that influences its performance is a lot, but silver powder is the material of forming the conductive silver paste most critical.Silver powder must be as far as possible little near single size, reunion degree as far as possible, have a high-tap density simultaneously.
If use the silver slurry for preparing like the said silver powder that forms as dispersant through interpolation aliphatic acid, surfactant etc. of the open communique No.10-88206 of Japan Patent to be printed on the base material; Can cause the silver slurry to be not easy to peel off, thereby make silver produce bubble in starching from web plate.As a result, certain situation can take place, promptly the film of sintering is inhomogeneous, thereby makes the resistance of said film change.Therefore, such plate is not suitable for printed circuit.Invention disclosed patent application on September 20 " preparation method of nano-scale silver powder " in 2000 the publication number CN1266761A of China national Department of Intellectual Property, this invention is that silver nitrate is dissolved in water, and adds ammoniacal liquor again and processes silver ammino solution; Slowly add the reducing solution that is made into by reducing agent and protective agent then, reducing agent is anti-ascorbic acid, hydrazine hydrate or borohydride sodium, and protective agent is polyvinylpyrrolidone (PCP), alkyl hydrosulfide (RSH), oleic acid or palmitic acid; Silver in the silver ammino solution is reduced into nano level silver powder; After filtering out silver powder, it is immersed in the oleic acid as passivator, removes by filter oleic acid; After the vacuum drying, promptly obtain nano-scale silver powder.Nano-scale silver powder stability, good dispersion that this inventive method makes, but technology is complicated, and suitability for industrialized production acquires a certain degree of difficulty.
Especially, silver powder use in anodal serigraphy for solar cell, and the silver powder used of the electric slurry of the base material electrode of LED display floater and circuit, and specific requirement is exactly: monodispersity is good, and powder reuniting is few, and tap density height and specific area are little.
Summary of the invention
The object of the invention is exactly to provide in order to overcome the defective that above-mentioned prior art exists that a kind of tap density is high, good, the smooth surface of monodispersity, and specific area is little and be easy to single preparation method who disperses the low reunion silver powder of high jolt ramming of large-scale production.
The object of the invention can be realized through following technical scheme:
Single preparation method who disperses the low reunion silver powder of high jolt ramming, with acid silver salt solution and the even hybrid reaction of mixing reducing solution that contains reducing agent, protective agent and surfactant, the gained deposition is single low reunion silver powder of high jolt ramming that disperses behind cleaning-drying.
Described acid silver salt solution can be any soluble silver salt, such as silver nitrate.The silver salt amount is 0.25-0.45mol/L.
The component of described mixing reducing solution and content are: reducing agent can be L-ascorbic acid, D-ascorbic acid and its esters, and used mole is 0.5-0.7 a times of silver ion mole; Protective agent can be any soluble potassium salt, and for example: potash, potassium nitrate, potassium sulfate etc., used mole is 10 of a silver ion mole
-2-10
-4Mole doubly; Surfactant can be a kind of in gelatin, polyethylene glycol (600-8000), ammonium stearate or other stearate, used quality be silver ion quality 0.001-0.8 doubly, last, will mix reducing solution pH and transfer to smaller or equal to 2.
Described hybrid reaction is meant: under the environment of stirring at low speed, mix, and the control reaction temperature reaction time 3-10 minute, treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 2-4 hour anyway at 20-50 ℃.
The container that relates in the described hybrid reaction all under 70-90 ℃, Na
3PO
480-100g/L, Na
2CO
3100-150g/L, NaOH 100-150g/L, H
2O
2Clean 15-25min in the solution of 20-50ml/L, clean with deionized water then.
Described cleaning-drying is meant: the precipitate with deionized water of hybrid reaction cleaned to electrical conductivity＜100us/cm, cleans 2-3 time with acetone or absolute alcohol again, and in air dry oven 30-40 ℃ at last, dry 24-36 hour.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
Preparing acid silver salt solution all is deionized pure water with mixing the used water of reducing solution.
Compared with prior art, the invention provides tap density is 5.0-5.5g/ml, and average middle particle diameter is the silver powder of 0.2-5um.Under laser particle analyzer test, its span is at 0.7-1.3, specific area 0.4-1.1m
2/ g, the obtained silver powder tap density height of the present invention, particle size dispersion narrow range, its particle sphericity are high, smooth surface, specific area is little and be easy to large-scale production.
Description of drawings
Fig. 1 is SEM * 5000 patterns of gained micron order silver powder of the present invention;
Fig. 2 is SEM * 12000 patterns of gained micron order silver powder of the present invention;
Fig. 3 is the laser particle size analysis result of gained micron order silver powder of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment 1
To used reaction with container, paddle etc., under 85 ℃, Na
3PO
480g/L, Na
2CO
3120g/L, NaOH 120g/L, H
2O
2Clean 15min in the solution of 30ml/L, clean with deionized water then.
Prepare acid silver salt solution, wherein silver nitrate 0.25mol/L.Preparation mixes reducing solution.L-ascorbic acid 0.13mol/L, polyethylene glycol (2000) 2.5 * 10
-4Mol/L, potassium nitrate 0.03g/L are mixed with the mixing reducing solution with deionized water.At last, will mix reducing solution pH and transfer to 1.In stirring at low speed mixing reducing solution, acid silver salt solution is evenly mixed with the mixing reducing solution react fast, control reaction temperature at 20 ℃, reaction time 5min.Reacted silver powder is carried out post processing.Treat that anyway the back sedimentation after 3 hours removes the supernatant reactant liquor, then the silver powder of deposition with washed with de-ionized water to electrical conductivity 20 μ s/cm, clean 2 times with absolute alcohol again.With the silver powder of cleaning in air dry oven 35 ℃, dry 26 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
1 of embodiment makes silver powder, tap density: 5.3g/ml specific area: 0.64m
2/ g D
501.8um very narrow size distribution, the SEM photo of the micron order silver powder for preparing is shown in Fig. 1-2, and grain size analysis is as shown in Figure 3.
Embodiment 2
To used reaction with container, paddle etc., under 90 ℃, Na
3PO
490g/L, Na
2CO
3100g/L, NaOH 130g/L, H
2O
2Clean 20min in the solution of 40ml/L, clean with deionized water then.
Prepare acid silver salt solution, wherein silver nitrate 0.30mol/L.Preparation mixes reducing solution.L-ascorbic acid 0.18mol/L, gelatin 3.0 * 10
-3Mol/L, potash 0.05g/L are mixed with the mixing reducing solution with deionized water.At last, will mix reducing solution pH and transfer to 0.5.In stirring at low speed mixing reducing solution, acid silver salt solution is evenly mixed with the mixing reducing solution react fast, control reaction temperature at 25 ℃, reaction time 6min.Reacted silver powder is carried out post processing.Treat that anyway the back sedimentation after 4 hours removes the supernatant reactant liquor, then the silver powder of deposition with washed with de-ionized water to electrical conductivity 35 μ s/cm, clean 1 time with absolute alcohol again.With the silver powder of cleaning in air dry oven 40 ℃, dry 30 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
2 of embodiment make silver powder, tap density: 5.2g/ml specific area: 0.73m
2/ g D
501.5um very narrow size distribution.
Embodiment 3
To used reaction with container, paddle etc., under 80 ℃, Na
3PO
4100g/L, Na
2CO
3130g/L, NaOH 150g/L, H
2O
2Clean 25min in the solution of 35ml/L, clean with deionized water then.
Prepare acid silver salt solution, wherein silver nitrate 0.40mol/L.Preparation mixes reducing solution.L-ascorbic acid 0.22mol/L, ammonium stearate 0.052mol/L, potassium sulfate 0.7g/L are mixed with the mixing reducing solution with deionized water.At last, will mix reducing solution pH and transfer to 0.3.In stirring at low speed mixing reducing solution, acid silver salt solution is evenly mixed with the mixing reducing solution react fast, control reaction temperature at 30 ℃, reaction time 8min.Reacted silver powder is carried out post processing.Treat that anyway the back sedimentation after 4 hours removes the supernatant reactant liquor, then the silver powder of deposition with washed with de-ionized water to electrical conductivity 50 μ s/cm, clean 2 times with absolute alcohol again.With the silver powder of cleaning in air dry oven 38 ℃, dry 32 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
3 of embodiment make silver powder, tap density: 5.4g/ml specific area: 0.80m
2/ g D
501.9um very narrow size distribution.
Embodiment 4
Single preparation method who disperses the low reunion silver powder of high jolt ramming; This method is 0.25mol/L liquor argenti nitratis ophthalmicus and the even hybrid reaction of mixing reducing solution that contains reducing agent L-ascorbic acid, protective agent potash and surfactant ammonium stearate with concentration; The used mole of reducing agent L-ascorbic acid is 0.5 times of silver ion mole, and the used mole of protective agent potash is 10 of a silver ion mole
-2, the used quality of surfactant ammonium stearate is a silver ion quality 0.001, mixing reducing solution pH value is 2; Under the environment of stirring at low speed, mix, and control reaction temperature at 20 ℃, 10 minutes reaction time; Treat that the back sedimentation reached its deposition with the supernatant reactant liquor after 2 hours anyway, to electrical conductivity＜100us/cm, clean 2 times with acetone or absolute alcohol again with washed with de-ionized water; In air dry oven 30 ℃ at last, dry 36 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder to be single low reunion silver powder of high jolt ramming that disperses.
The container that relates in the hybrid reaction all under 70 ℃, utilizes the Na of concentration for 80g/L
3PO
4, 100g/L Na
2CO
3, the NaOH of 100g/L, 20ml/L H
2O
2Solution in clean 25min, clean with deionized water then, preparing acid silver salt solution all is deionized pure water with mixing the used water of reducing solution.
Embodiment 5
Single preparation method who disperses the low reunion silver powder of high jolt ramming; With concentration is the liquor argenti nitratis ophthalmicus and the even hybrid reaction of mixing reducing solution that contains reducing agent D-ascorbic acid, protective agent potassium sulfate and surfactant polyethylene of 0.45mol/L; The used mole of reducing agent D-ascorbic acid is 0.7 times of silver ion mole, and the used mole of protective agent potassium sulfate is 10 of a silver ion mole
-4, the used quality of surfactant polyethylene is a silver ion quality 0.8, mixing reducing solution pH value is 1; Under the environment of stirring at low speed, mix, and control reaction temperature at 50 ℃, 3 minutes reaction time; Treat that the back sedimentation reached its deposition with the supernatant reactant liquor after 4 hours anyway, to electrical conductivity＜100us/cm, clean 3 times with acetone or absolute alcohol again with washed with de-ionized water; In air dry oven 40 ℃ at last, dry 24 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder to be single low reunion silver powder of high jolt ramming that disperses.
The container that relates in the hybrid reaction all under 90 ℃, utilizes the Na of concentration for 100g/L
3PO
4, 150g/L Na
2CO
3, the NaOH of 150g/L, 50ml/L H
2O
2Solution in clean 15min, clean with deionized water then, preparing acid silver salt solution all is deionized pure water with mixing the used water of reducing solution.
The foregoing description provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Claims (10)
1. a list disperses high jolt ramming to hang down the preparation method of reunion silver powder; It is characterized in that; This method be with acid silver salt solution with contain reducing agent, protective agent and surfactant mix the even hybrid reaction of reducing solution, the gained sediment is single low reunion silver powder of high jolt ramming that disperses behind cleaning-drying.
2. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1 is characterized in that what adopt in the described acid silver salt solution is soluble silver salt.
3. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 2 is characterized in that described soluble silver salt comprises silver nitrate.
4. according to a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming described in claim 1 or 2 or 3, it is characterized in that the concentration of described acid silver salt solution is 0.25-0.45mol/L.
5. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1; It is characterized in that; Reducing agent in the described mixing reducing solution is L-ascorbic acid, D-ascorbic acid or its esters, and the reducing agent mole is 0.5-0.7 a times of silver ion mole in the acid silver salt solution; Described protective agent is a soluble potassium salt, comprises potash, potassium nitrate or potassium sulfate, and protectant mole is 10-2-10-4 a times of silver ion mole in the acid silver salt solution; Described surfactant comprises gelatin, polyethylene glycol, ammonium stearate or stearate, and the quality of surfactant is that silver ion quality 0.001-0.8 is doubly in the acid silver salt solution.
6. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1 is characterized in that the pH of described mixing reducing solution is smaller or equal to 2.
7. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1; It is characterized in that; Hybrid reaction is meant under the environment of stirring at low speed mixes; The control reaction temperature reaction time 3-10 minute, reaches its deposition with the supernatant reactant liquor after sedimentation 2-4 hour then at 20-50 ℃.
8. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1 is characterized in that the container that hybrid reaction adopts all under 70-90 ℃, utilizes the Na of concentration for 80-100g/L
3PO
4, 100-150g/L Na
2CO
3, the NaOH of 100-150g/L, the H of 20-50ml/L
2O
2Solution cleans 15-25min, cleans with deionized water then.
9. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1; It is characterized in that, cleaning-drying be sediment with hybrid reaction with washed with de-ionized water to electrical conductivity＜100us/cm, clean 2-3 time with acetone or absolute alcohol again; In air dry oven 30-40 ℃ then; Dry 24-36 hour, at last dried silver powder is beaten powder, cross screen cloth and become powder to get final product.
10. a kind of single preparation method who disperses the low reunion silver powder of high jolt ramming according to claim 1 is characterized in that preparing acid silver salt solution all is deionized pure water with mixing the used water of reducing solution.
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| 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 |
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| CN107876799A (en) * | 2017-12-18 | 2018-04-06 | 西安宏星电子浆料科技有限责任公司 | High-tap density low specific surface area super fine silver powder and preparation method thereof |
| CN108672718A (en) * | 2018-06-07 | 2018-10-19 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of the spherical silver powder of high specific area and its silver powder obtained |
| CN111360281A (en) * | 2020-05-11 | 2020-07-03 | 河南金渠银通金属材料有限公司 | Excellent conductive silver powder and preparation method thereof |
| CN114082976A (en) * | 2021-11-10 | 2022-02-25 | 电子科技大学 | Preparation method of high-crystallinity nano silver powder |
| CN115740480A (en) * | 2022-11-03 | 2023-03-07 | 云南驰宏锌锗股份有限公司 | Preparation method of superfine spherical silver powder |
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Application publication date: 20120208 |