CN102554265A - Preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size - Google Patents
Preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size Download PDFInfo
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- CN102554265A CN102554265A CN2012100719858A CN201210071985A CN102554265A CN 102554265 A CN102554265 A CN 102554265A CN 2012100719858 A CN2012100719858 A CN 2012100719858A CN 201210071985 A CN201210071985 A CN 201210071985A CN 102554265 A CN102554265 A CN 102554265A
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Abstract
The invention relates to a preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size. The preparation method comprises uniformly mixing an acidic silver salt solution and a mixed reducing solution containing a reducing agent, a dispersing agent and a stabilizing agent, precipitating, washing and drying to obtain the mono-dispersed highly crystalline silver powder with adjustable particle size, wherein the particle size of the silver powder can be adjusted by adjusting the amount of the dispersing agent and the stabilizing agent. In comparison with the prior art, the silver powder has an adjustable particle size, and D50 of the silver powder can be controlled to a range close to 0.5 mum, 1.0 mum, and 2.5 mum. Meanwhile, the silver powder has the advantages of narrow particle size distribution range, high tap density, high particle sphericity, smooth surface, and small specific surface area, and is easy for large-scale production.
Description
Technical field
The present invention relates to a kind of material and method of field of electrical components, specifically is the preparation method that a kind of adjustable particle diameter list disperses high crystallization silver powder.
Background technology
The preparation of high-purity, high dispersive, superfines is one of focus of present material scientific research.In electronics industry, silver powder is widely used in makes various electrocondution slurries, is used for the internal and external electrode of printed circuit and electronic component.Owing to do development of electronic technology, the precise treatment of printed circuit and electronic component and miniaturization require silver powder to develop to high-purity, high dispersive and ultra-fine direction, and be spherical in shape as far as possible or type spherical in shape.
The preparation method of silver powder comprises vapor phase method, solid phase method and liquid phase method.The investment of vapor phase method is big, energy consumption is high, productive rate is low; The particle diameter of the silver powder of solid phase method preparation is bigger than normal and particle size distribution range is wide, generally is applied to the preparation of ceramic powder, and uses less in the industrial preparation of metal-powder; The liquid phase method technical process is fairly simple, and powder granule size and shape are controlled easily, is the common method of low-cost at present preparation silver powder.Internal and external electrode silver slurry for preparation printed circuit and electronic component needs with multiple particle diameter (D
50) silver powder carry out composite, thereby just can effectively reduce the resistance of sintering rear electrode.Simultaneously through this composite, can make the electrode behind the sintering on microcosmic, form a fixed structure.This structural electrode reduces the content of used silver powder when can keep high conductivity, can reduce silver slurry cost greatly.
Retrieval through to prior art finds that if use invention disclosed patent application on September 20 " preparation method of nano-scale silver powder " in 2000 the publication number CN1266761A of Intellectual Property in China office, this invention is that silver nitrate is dissolved in water; Add ammoniacal liquor again and process 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.If use open patent of invention " high-tap density ball shape silver powder and preparation thereof and application " publication number CN102172777A in Intellectual Property in China office on September 7th, 2011; This invention is with silver nitrate-ammonia water mixture and the even hybrid reaction of mixing reducing solution that contains L-ascorbic acid, protective agent and surfactant, and the gained deposition is the high-tap density ball shape silver powder behind cleaning-drying.This invents, and obtained silver powder tap density is high, dispersion range is narrow, its particle sphericity is high.But the particle diameter of output silver powder is single, is not suitable for high-resolution, the silver slurry preparation of high conductivity.
Summary of the invention
The object of the invention is exactly to provide a kind of technology is simple, cost is low adjustable particle diameter list to disperse the preparation method of high crystallization silver powder in order to overcome the defective that above-mentioned prior art exists.
The object of the invention can be realized through following technical scheme: a kind of adjustable particle diameter list disperses the preparation method of high crystallization silver powder; It is characterized in that; With acid silver salt solution and the even hybrid reaction of mixing reducing solution that contains reducing agent, dispersant and stabilizing agent; Simultaneously, through regulating the consumption of dispersant and stabilizing agent, the gained deposition is adjustable particle diameter list and disperses high crystallization silver powder behind cleaning-drying.
Described acid silver salt solution is silver carbonate solution or liquor argenti nitratis ophthalmicus, and wherein the silver salt amount is 0.3-0.6mol/L;
The component of described mixing reducing solution and content are: the used mole of reducing agent be the silver ion mole 0.5-0.7 doubly, the used quality of stabilizing agent be the silver ion quality 0.02-0.008 doubly, the used mole of dispersant be the silver ion mole 0.01-0.8 doubly, the pH value of described mixing reducing solution is less than or equal to 2.
Described reducing agent is one or more of D-ascorbic acid, L-ascorbic acid and its esters; Described stabilizing agent is a kind of in potash, potassium nitrate or the potassium sulfate; Described dispersant is a kind of in PVP, oleic acid, the ammonium stearate.
The particle diameter of the consumption adjusting silver powder through regulating dispersant and stabilizing agent, the wherein relation such as the following table of dispersant and protective agent consumption and silver powder particle size range:
Described hybrid reaction is meant: under stirring at low speed, the control reaction temperature is 5-40 ℃, reaction time 5-10 minute, treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 2-4 hour anyway.
The speed of described stirring at low speed is 300-500rmp.
The container that relates in the described hybrid reaction all under temperature 70-90 ℃, cleans 10-20min in cleaning fluid, clean with deionized water then, and described cleaning fluid is Na
3PO
490-100g/L, Na
2CO
3120-150g/L, NaOH 125-150g/L, H
2O
2The mixed liquor of 20-50ml/L.
Described deposition is meant through cleaning-drying: the precipitate with deionized water of hybrid reaction cleaned to electrical conductivity＜50us/cm, cleans 2-3 time with acetone or absolute alcohol again, and in air dry oven 40-50 ℃ at last, dry 24-36 hour; At last dried silver powder is beaten powder, cross screen cloth and can become powder.
Prepare acid silver salt solution and mix reducing solution, used water all is deionized pure water.
Compared with prior art, the adjustable grain of the silver powder that the present invention makes, D
50Can be controlled near 0.5 μ m, 1.0 μ m, the 2.5 μ m.Simultaneously, particle size dispersion narrow range, tap density are high, sphericity is high, smooth surface, and specific area is little and be easy to large-scale production.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment 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.
Embodiment 1
To used reaction with container, paddle etc., under 85 ℃, Na
3PO
495g/L, Na
2CO
3120g/L, NaOH130g/L, H
2O
2Clean 15min in the solution of 25ml/L, clean with deionized water then.
Prepare acid silver salt solution, wherein silver nitrate 0.30mol/L.Preparation mixes reducing solution.L-ascorbic acid 0.16mol/L, PVP 0.009mol/L, potassium nitrate 0.60g/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 8min.Reacted silver powder is carried out post processing.Treat that anyway the back sedimentation after 2 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 40 ℃, dry 24 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
1 of embodiment makes silver powder, tap density: 5.2g/ml specific area: 0.46m
2/ g D
502.2um very narrow size distribution.
Embodiment 2
To used reaction with container, paddle etc., under 90 ℃, Na
3PO
498g/L, Na
2CO
3130g/L, NaOH140g/L, H
2O
2Clean 20min in the solution of 20ml/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, oleic acid 0.02mol/L, potash 0.35g/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 25 ℃, reaction time 6min.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 35 μ s/cm, clean 1 time with absolute alcohol again.With the silver powder of cleaning in air dry oven 50 ℃, dry 50 hours.At last dried silver powder is beaten powder, cross screen cloth and can become powder.
2 of embodiment make silver powder, tap density: 5.3g/ml specific area: 0.56m
2/ g D
501.1um very narrow size distribution.
Embodiment 3
To used reaction with container, paddle etc., under 80 ℃, Na
3PO
4100g/L, Na
2CO
3130g/L, NaOH150g/L, H
2O
2Clean 15min in the solution of 25ml/L, clean with deionized water then.
Prepare acid silver salt solution, wherein silver nitrate 0.35mol/L.Preparation mixes reducing solution.L-ascorbic acid 0.18mol/L, ammonium stearate 0.025mol/L, potassium sulfate 0.8g/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 30 ℃, reaction time 10min.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 20 μ s/cm, clean 2 times with absolute alcohol again.With the silver powder of cleaning in air dry oven 45 ℃, 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: 4.9g/ml, specific area: 0.80m
2/ g, D
500.5um very narrow size distribution.
Embodiment 4
Used reaction with container, paddle etc., all under 70 ℃ of temperature, is cleaned 20min in cleaning fluid, clean with deionized water then, described cleaning fluid is Na
3PO
490g/L, Na
2CO
3120g/L, NaOH125g/L, H
2O
2The mixed liquor of 20ml/L.
A kind of adjustable particle diameter list disperses the preparation method of high crystallization silver powder; With deionized pure water preparation silver carbonate solution and mixing reducing solution; Silver salt amount in the silver carbonate solution is 0.3mol/L; The component and the content that mix reducing solution are: the used mole of reducing agent D-ascorbic acid be 0.5 times of the silver ion mole, the used quality of stabilizing agent potash be the silver ion quality 0.01-0.25 doubly, the used mole of dispersant PVP be the silver ion mole 0.02-0.04 doubly, the pH value of described mixing reducing solution is less than or equal to 2; With silver carbonate solution with mix reducing solution under stirring at low speed (300-500rmp); At 5 ℃, hybrid reaction 10 minutes treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 2 hours anyway; Precipitate with deionized water is cleaned to electrical conductivity＜50us/cm; Clean 2 times with acetone or absolute alcohol again, in air dry oven 50 ℃ at last, dry 24 hours; At last dried silver powder is beaten powder, cross screen cloth and can become powder, gained silver powder particle size range is 2.0-2.5 μ m.
Embodiment 5
Used reaction with container, paddle etc., all under 90 ℃ of temperature, is cleaned 10min in cleaning fluid, clean with deionized water then, described cleaning fluid is Na
3PO
4100g/L, Na
2CO
3150g/L, NaOH150g/L, H
2O
2The mixed liquor of 50ml/L.
A kind of adjustable particle diameter list disperses the preparation method of high crystallization silver powder; With deionized pure water preparation silver carbonate solution and mixing reducing solution; Silver salt amount in the silver carbonate solution is 0.6mol/L; The component and the content that mix reducing solution are: the used mole of reducing agent D-ascorbic acid be 0.6 times of the silver ion mole, the used quality of stabilizing agent potash be the silver ion quality 0.25-0.6 doubly, the used mole of dispersant ammonium stearate be the silver ion mole 0.04-0.06 doubly, the pH value of described mixing reducing solution is less than or equal to 2; With silver carbonate solution with mix reducing solution under stirring at low speed (300-500rmp); At 40 ℃, hybrid reaction 5 minutes treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 4 hours anyway; Precipitate with deionized water is cleaned to electrical conductivity＜50us/cm; Clean 3 times with acetone or absolute alcohol again, in air dry oven 40 ℃ at last, dry 36 hours; At last dried silver powder is beaten powder, cross screen cloth and can become powder, gained silver powder particle size range is 0.9-1.2 μ m.
Embodiment 6
Used reaction with container, paddle etc., all under 80 ℃ of temperature, is cleaned 15min in cleaning fluid, clean with deionized water then, described cleaning fluid is Na
3PO
495g/L, Na
2CO
3130g/L, NaOH140g/L, H
2O
2The mixed liquor of 30ml/L.
A kind of adjustable particle diameter list disperses the preparation method of high crystallization silver powder; With deionized pure water preparation silver carbonate solution and mixing reducing solution; Silver salt amount in the silver carbonate solution is 0.5mol/L; The component and the content that mix reducing solution are: the used mole of reducing agent D-ascorbic acid be 0.7 times of the silver ion mole, the used quality of stabilizing agent potash be the silver ion quality 0.6-0.8 doubly, the used mole of dispersant oleic acid be the silver ion mole 0.06-0.08 doubly, the pH value of described mixing reducing solution is less than or equal to 2; With silver carbonate solution with mix reducing solution under stirring at low speed (300-500rmp); At 30 ℃, hybrid reaction 80 minutes treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 3 hours anyway; Precipitate with deionized water is cleaned to electrical conductivity＜50us/cm; Clean 3 times with acetone or absolute alcohol again, in air dry oven 50 ℃ at last, dry 30 hours; At last dried silver powder is beaten powder, cross screen cloth and can become powder, gained silver powder particle size range is 0.5-0.8 μ m.
Claims (9)
1. an adjustable particle diameter list disperses the preparation method of high crystallization silver powder; It is characterized in that; With acid silver salt solution and the even hybrid reaction of mixing reducing solution that contains reducing agent, dispersant and stabilizing agent; Simultaneously, through regulating the consumption of dispersant and stabilizing agent, the gained deposition is adjustable particle diameter list and disperses high crystallization silver powder behind cleaning-drying.
2. a kind of adjustable particle diameter list according to claim 1 disperses the preparation method of high crystallization silver powder, it is characterized in that, described acid silver salt solution is silver carbonate solution or liquor argenti nitratis ophthalmicus, and wherein the silver salt amount is 0.3-0.6mol/L;
The component of described mixing reducing solution and content are: the used mole of reducing agent be the silver ion mole 0.5-0.7 doubly, the used quality of stabilizing agent be the silver ion quality 0.02-0.008 doubly, the used mole of dispersant be the silver ion mole 0.01-0.8 doubly, the pH value of described mixing reducing solution is less than or equal to 2.
3. a kind of adjustable particle diameter list according to claim 1 and 2 disperses the preparation method of high crystallization silver powder, it is characterized in that, described reducing agent is one or more of D-ascorbic acid, L-ascorbic acid and its esters; Described stabilizing agent is a kind of in potash, potassium nitrate or the potassium sulfate; Described dispersant is a kind of in PVP, oleic acid, the ammonium stearate.
4. a kind of adjustable particle diameter list according to claim 1 disperses the preparation method of high crystallization silver powder; It is characterized in that; The particle diameter of the consumption adjusting silver powder through regulating dispersant and stabilizing agent, the wherein relation such as the following table of dispersant and protective agent consumption and silver powder particle size range:
5. a kind of adjustable particle diameter list according to claim 1 disperses the preparation method of high crystallization silver powder; It is characterized in that; Described hybrid reaction is meant: under stirring at low speed; The control reaction temperature is 5-40 ℃, reaction time 5-10 minute, treats that the back sedimentation reached its deposition with the supernatant reactant liquor after 2-4 hour anyway.
6. a kind of adjustable particle diameter list according to claim 5 disperses the preparation method of high crystallization silver powder, it is characterized in that, the speed of described stirring at low speed is 300-500rmp.
7. a kind of adjustable particle diameter list according to claim 1 disperses the preparation method of high crystallization silver powder; It is characterized in that the container that relates in the described hybrid reaction all under temperature 70-90 ℃, cleans 10-20min in cleaning fluid; Clean with deionized water then, described cleaning fluid is Na
3PO
490-100g/L, Na
2CO
3120-150g/L, NaOH 125-150g/L, H
2O
2The mixed liquor of 20-50ml/L.
8. the preparation method who disperses high crystallization silver powder based on the described a kind of adjustable particle diameter list of claim 1; It is characterized in that; Described deposition is meant through cleaning-drying: the precipitate with deionized water of hybrid reaction is cleaned to electrical conductivity＜50us/cm; Clean 2-3 time with acetone or absolute alcohol again, in air dry oven 40-50 ℃ at last, dry 24-36 hour; At last dried silver powder is beaten powder, cross screen cloth and can become powder.
9. a kind of adjustable particle diameter list according to claim 1 disperses the preparation method of high crystallization silver powder, it is characterized in that, prepares acid silver salt solution and mixes reducing solution, and used water all is deionized pure water.
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| CN103831444A (en) * | 2014-03-11 | 2014-06-04 | 上海交通大学 | Preparation method for high-crystallized flake silver powders |
| CN103978226A (en) * | 2014-05-26 | 2014-08-13 | 熊仕显 | Micro nano silver-based material preparation method and micro nano silver-based material |
| CN104096850A (en) * | 2014-08-12 | 2014-10-15 | 天津市职业大学 | Method for preparing superfine spherical silver powder by reducing silver-ammonia complex with aminophenol |
| CN104148665A (en) * | 2014-07-22 | 2014-11-19 | 西北大学 | Preparation method of crystalized sliver powder |
| CN104646683A (en) * | 2015-02-28 | 2015-05-27 | 湖南汇通科技有限责任公司 | Spherical silver powder with controllable granularity and preparation method thereof |
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| TWI508799B (en) * | 2012-12-06 | 2015-11-21 | China Steel Corp | A Method for Synthesis of Silver Powder with Adjustable Particle Size |
| CN103394701A (en) * | 2013-07-16 | 2013-11-20 | 宁波晶鑫电子材料有限公司 | Method for preparing superfine sliver powder uniform and concentrated in particle size |
| CN103394701B (en) * | 2013-07-16 | 2016-03-02 | 宁波晶鑫电子材料有限公司 | The preparation method of the super fine silver powder that a kind of epigranular is concentrated |
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| CN103978226A (en) * | 2014-05-26 | 2014-08-13 | 熊仕显 | Micro nano silver-based material preparation method and micro nano silver-based material |
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| CN104148665A (en) * | 2014-07-22 | 2014-11-19 | 西北大学 | Preparation method of crystalized sliver powder |
| CN104096850A (en) * | 2014-08-12 | 2014-10-15 | 天津市职业大学 | Method for preparing superfine spherical silver powder by reducing silver-ammonia complex with aminophenol |
| CN104096850B (en) * | 2014-08-12 | 2017-10-10 | 天津市职业大学 | The method that silver ammonia complex prepares superfine spherical silver powder is reduced with para-aminophenol |
| CN104646683A (en) * | 2015-02-28 | 2015-05-27 | 湖南汇通科技有限责任公司 | Spherical silver powder with controllable granularity and preparation method thereof |
| CN105268990A (en) * | 2015-11-09 | 2016-01-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing ultrafine silver powder through ultrasonic decentralized processing and inert atmosphere protection |
| CN110114175A (en) * | 2016-10-13 | 2019-08-09 | LS-Nikko铜制炼株式会社 | High temperature sintering type silver powder and its manufacturing method |
| CN110114175B (en) * | 2016-10-13 | 2022-06-14 | LS-Nikko铜制炼株式会社 | High-temperature sintered silver powder and method for producing same |
| CN108746664A (en) * | 2018-09-10 | 2018-11-06 | 河南金渠银通金属材料有限公司 | A kind of high oil absorption rate photovoltaic silver powder and the preparation method and application thereof |
| CN110586929A (en) * | 2019-09-23 | 2019-12-20 | 西安汇创贵金属新材料研究院有限公司 | Auxiliary reagent suitable for preparing spherical micron silver powder |
| CN111451521A (en) * | 2020-03-30 | 2020-07-28 | 长春黄金研究院有限公司 | Method for preparing high-tap-density spherical silver powder by chemical method |
| CN111451521B (en) * | 2020-03-30 | 2022-06-03 | 长春黄金研究院有限公司 | Method for preparing high-tap-density spherical silver powder by chemical method |
| CN111331150A (en) * | 2020-04-07 | 2020-06-26 | 郑州卓而泰新材料科技有限公司 | Preparation method of high-dispersion spheroidal superfine silver powder with controllable particle size |
| 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 |
| 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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