CN104148665A - Preparation method of crystalized sliver powder - Google Patents
Preparation method of crystalized sliver powder Download PDFInfo
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- CN104148665A CN104148665A CN201410346916.2A CN201410346916A CN104148665A CN 104148665 A CN104148665 A CN 104148665A CN 201410346916 A CN201410346916 A CN 201410346916A CN 104148665 A CN104148665 A CN 104148665A
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Abstract
The invention discloses a preparation method of crystalized sliver powder. The preparation method includes the steps of dissolving dispersant and silver nitrate in deionized water to obtain first solution, dissolving dispersant, surfactant, ascorbic acid and pH modifier in water to obtain second solution, adding the first solution into the second solution or the second solution into the first solution while stirring, adding the pH modifier to maintain pH of a reaction system stable during the whole course, controlling the temperature of the reaction system to be 25-45 DEG C, and performing washing and drying to obtain the crystalized sliver powder after reaction is over. By the use of the preparation method, the problem in mononuclear crystallization of the slivered powder is effectively solved; the tap density of the prepared sliver powder can be larger than 5.5g/cm<3> per specification.
Description
Technical field
The present invention relates to a kind of preparation method of crystallization silver powder, in particular to the preparation method of high-tap density crystallization silver powder.
Technical background
In recent years, electronics industry develop rapidly, particularly, along with the developing rapidly of heliotechnics, conductive silver paste receives much concern as producing the fundamental sum key function material of various electronic devices and components, and following new electronic device and production Technology are by the new silver powder silver slurry technology of needs.In solar energy electronic slurry, silver powder content surpasses 90%, and the quality of quality of cathode silver directly affects the electrical property of slurry.At present, China has become the first producing country of world's solar-energy photo-voltaic cell, the most of material of China solar photovoltaic assembly has been realized production domesticization, however front electrode silver plasm material still by offshore company, monopolized, one of its reason is that China still can not production high-performance silver powder.Research and development high-performance silver powder (as: high-tap density, single dispersion, particle diameter, pattern were controlled) is the needs of silver powder industry development.
Chemical reduction method is the most common silver powder method of preparing in enormous quantities at present.And the key point of chemical preparation silver powder is how to control pattern, particle diameter and the dispersiveness of silver powder.Patent application 200680024526.7 discloses the preparation method of a kind of high crystallization silver powder and this high crystallization silver powder, and primary particle size is 0.07 μ m ~ 4.5 μ m, but this silver powder on-monocrystalline nucleation, degree of crystallinity is not high, particle diameter distributes wide, and tap density is not high, is difficult to meet the requirement of solar energy silver paste.Patent application 201310036975.5 discloses a kind of preparation method of high jolt ramming list dispersible silver powder, by having added micro-base metal to lure agent to mix in course of reaction, use, in preparation process, efficiently solve silver powder monokaryon crystallisation problems, can prepare single specification silver powder tap density and can be greater than 5.5g/cm
3, but base metal lures the introducing of agent in final silver powder, to introduce impurity, thus affect silver powder performance.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of high-tap density mono-dispersed and crystalline silver powder, it is spherical that this silver powder microscopic appearance is polyhedron class, can meet middle and high end silver slurry demand, under high solids content, printing-sintering has low shrinkage factor, thereby reaches high printing precision.
The present invention seeks to be achieved through the following technical solutions:
A preparation method for crystallization silver powder, comprises the following steps:
(1) silver nitrate and dispersant are dissolved in to deionized water preparation the 1st aqueous solution;
(2) by the water-soluble preparation of dispersant, surfactant, ascorbic acid and pH adjusting agent the 2nd aqueous solution;
(3) under agitation in the 2nd aqueous solution, add the 1st aqueous solution or add the 2nd aqueous solution in the 1st aqueous solution, in course of reaction, adding pH adjusting agent, to maintain reaction system pH be 0.7 ~ 2.0, reaction at 25 ℃ ~ 45 ℃, reaction finishes by the dry crystallization silver powder that obtains of washing;
Described dispersant is selected from gelatin, polyvinylpyrrolidone, 1-METHYLPYRROLIDONE, polyvinyl alcohol, triethanolamine, trisodium citrate, gum arabic;
Described surfactant is selected from oleic acid, linoleic acid, myristic acid, laurate, palmitic acid, stearic acid.
The pH adjusting agent of adding in above-mentioned steps (2) and step (3) is selected from nitric acid, acetic acid, NaOH, ammoniacal liquor.
Above-mentioned dispersant dosage is 1 ~ 25g/L, and wherein in the 1st aqueous solution and the 2nd aqueous solution, adding mass ratio is 1:30～30:1.
In step (1), silver nitrate concentration is 50～200g/L.
In step (2), surfactant addition is 1～5% of silver nitrate quality; Ascorbic acid addition is for reducing 1.0 ~ 1.5 times of theoretical use amount of silver nitrate completely, and the concentration of ascorbic acid is 50～150g/L.
In step (3), mixing speed is 100 ~ 200r/min, and the reaction time is 10 ~ 40 minutes.
The present invention has the following advantages:
(1) the present invention is in course of reaction, by adding pH adjusting agent to maintain the stable of reaction system pH.Other conditions are constant, compare high pH, and ascorbic acid has lower reducing power under low pH, thereby the silver-colored nucleus that initial reaction stage forms can, in the later stage by crystal orientation growth, solve silver powder monokaryon crystallisation problems;
(2) the silver powder microscopic appearance preparing is that polyhedron class is spherical, has high tap density, good dispersed and good sintering character.Adapt to that this solid content of similar solar cell electric slurry is high, printing precision is high, shrinkage factor requires low silver paste, after sintering film forming, there is good electrical property;
(3) by regulating dispersant in the 1st and the 2nd aqueous solution, coordinate suitable surfactant and reaction temperature, make the crystallization silver powder particle size that makes adjustable, dispersion, good uniformity;
(4) the single specification tap density of crystal silver powder that prepared by the present invention can be greater than 5.5g/cm
3, by controlled condition, can prepare the different size list dispersible silver powder of 0.2 ~ 4 μ m;
(5) technique of the present invention is simple, the equal environmental friendliness of all reagent, and the crystal silver powder good stability of preparation, is easy to industrial production and amplifies.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the embodiment of the present invention 1 gained silver powder;
Fig. 2 is the SEM figure of the embodiment of the present invention 2 gained silver powder;
Fig. 3 is the SEM figure of the embodiment of the present invention 3 gained silver powder.
The specific embodiment
Below in conjunction with the specific embodiment, the preparation method of crystallization silver powder is further described.
Embodiment 1
In 30L deionized water, add 5kg silver nitrate, 40g polyvinylpyrrolidone (PVP), stir liquid temperature is heated to 30 ℃, make the 1st aqueous solution.Take 3.3kg ascorbic acid and add in 35L deionized water, add 800g polyvinylpyrrolidone (PVP), 50g oleic acid, adding nitric acid adjustment pH is 0.8, stirs liquid temperature is heated to 30 ℃, obtains the 2nd aqueous solution.Under agitation, in 30min, the 1st aqueous solution is added in the 2nd aqueous solution, in whole process, by adding ammoniacal liquor, maintain reaction system pH 0.8.In course of reaction, controlling temperature of reaction system is 30 ℃, and mixing speed is 120r/min.After completion of the reaction, continue to stir 15min.Standing after stopping stirring, make silver ion sedimentation, then, and elimination reactant liquor, washing, 70 ℃ of oven dry, obtain crystallization silver powder (see figure 1), gained silver powder tap density 5.35g/cm
3, average grain diameter 2.1 μ m.
Embodiment 2
In 40L deionized water, add 5kg silver nitrate, 40g gelatin, stir liquid temperature is heated to 35 ℃, make the 1st aqueous solution.Take 3.1kg ascorbic acid and add in 45L deionized water, add 100g gelatin, 100g oleic acid, adding nitric acid adjustment pH is 1.2, stirs liquid temperature is heated to 35 ℃, obtains the 2nd aqueous solution.Under agitation, in 30min, the 1st aqueous solution is added in the 2nd aqueous solution, in whole process, by adding ammoniacal liquor, maintain reaction system pH 1.0.In course of reaction, controlling temperature of reaction system is 35 ℃, and mixing speed is 150r/min.After completion of the reaction, continue to stir 15min.Standing after stopping stirring, make silver ion sedimentation, then, and elimination reactant liquor, washing, 70 ℃ of oven dry, obtain crystallization silver powder (see figure 2), gained silver powder tap density 5.70g/cm
3, average grain diameter 1.4 μ m.
Embodiment 3
In 50L deionized water, add 5kg silver nitrate, 1kg polyvinylpyrrolidone (PVP), stir liquid temperature is heated to 45 ℃, make the 1st aqueous solution.Take 3.1kg ascorbic acid and add in 50L deionized water, add 800g polyvinylpyrrolidone (PVP), 100g gelatin, 100g oleic acid, adding nitric acid adjustment pH is 1.5, stirs liquid temperature is heated to 45 ℃, obtains the 2nd aqueous solution.Under agitation, under stirring, in the 1st aqueous solution, add the 2nd aqueous solution in 15min, in whole process, by adding ammoniacal liquor, maintain reaction system pH 1.5.In course of reaction, controlling temperature of reaction system is 45 ℃, and mixing speed is 200r/min.After completion of the reaction, continue to stir 15min.Standing after stopping stirring, make silver ion sedimentation, then, and elimination reactant liquor, washing, 70 ℃ of oven dry, obtain crystallization silver powder (see figure 3), gained silver powder tap density 4.5g/cm
3, average grain diameter 0.4 μ m.
Comparative example 1
Comparative example 1 and embodiment 1 similar process, difference is, and with ammoniacal liquor, regulating reduction system (the 2nd aqueous solution) pH is 4.0, and in course of reaction, controlling reaction system pH is 3.9 ~ 4.1, and gained silver powder characteristic is in Table 1.
When comparative example 1 reacts under higher pH, compare the embodiment 1 of low pH reaction, it makes silver powder particle diameter wider distribution, and small particle diameter silver powder increases, and silver powder is reunited seriously simultaneously, and tap density is lower, is difficult to actual use, and design parameter is in Table 1.
Comparative example 2
Comparative example 2 and embodiment 2 similar process, difference is, and silver nitrate system in comparative example 2 (the 1st aqueous solution) does not add dispersant gelatin, and gained silver powder characteristic is in Table 2.
Silver nitrate system in comparative example 2 (the 1st aqueous solution) does not add dispersant gelatin, and it makes silver powder particle diameter and becomes large, and inhomogeneities increases, and dispersed poor, design parameter is in Table 2.
Comparative example 3
Comparative example 3 and embodiment 3 similar process, difference is, and comparative example 3 does not add pH adjusting agent in course of reaction, and gained silver powder characteristic is in Table 3.
Initial pH is identical with comparative example 3 for comparative example's 3 reaction system, and difference is that in comparative example's 3 courses of reaction, not controlling pH stablizes, with embodiment 3 contrasts, it makes silver powder particle diameter and enlarges markedly, tap density is lower, is difficult to actual use, and design parameter is in Table 3.
Claims (7)
1. a preparation method for crystallization silver powder, is characterized in that comprising the following steps:
(1) silver nitrate and dispersant are dissolved in to deionized water preparation the 1st aqueous solution;
(2) by the water-soluble preparation of dispersant, surfactant, ascorbic acid and pH adjusting agent the 2nd aqueous solution;
(3) under agitation in the 2nd aqueous solution, add the 1st aqueous solution or add the 2nd aqueous solution in the 1st aqueous solution, in course of reaction, adding pH adjusting agent, to maintain reaction system pH be 0.7 ~ 2.0, reaction at 25 ℃ ~ 45 ℃, reaction finishes by the dry crystallization silver powder that obtains of washing;
Described dispersant is selected from gelatin, polyvinylpyrrolidone, 1-METHYLPYRROLIDONE, polyvinyl alcohol, triethanolamine, trisodium citrate, gum arabic;
Described surfactant is selected from oleic acid, linoleic acid, myristic acid, laurate, palmitic acid, stearic acid.
2. the preparation method of crystallization silver powder according to claim 1, is characterized in that: the pH adjusting agent of adding in described step (2) and step (3) is selected from nitric acid, acetic acid, NaOH, ammoniacal liquor.
3. the preparation method of crystallization silver powder according to claim 1, is characterized in that: dispersant dosage is 1 ~ 25g/L, and wherein in the 1st aqueous solution and the 2nd aqueous solution, adding mass ratio is 1:30～30:1.
4. according to the preparation method of one of any described crystallization silver powder of claims 1 to 3, it is characterized in that: in step (1), silver nitrate concentration is 50～200g/L.
5. according to the preparation method of one of any described crystallization silver powder of claims 1 to 3, it is characterized in that: in step (2), surfactant addition is 1～5% of silver nitrate quality.
6. according to the preparation method of one of any described crystallization silver powder of claims 1 to 3, it is characterized in that: in step (2), ascorbic acid addition is for reducing 1.0 ~ 1.5 times of theoretical use amount of silver nitrate completely, and the concentration of ascorbic acid is 50～150g/L.
7. according to the preparation method of one of any described crystallization silver powder of claims 1 to 3, it is characterized in that: in step (3), mixing speed is 100 ~ 200r/min, and the reaction time is 10 ~ 40 minutes.
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| CN105252014A (en) * | 2015-10-30 | 2016-01-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing superfine silver powder in alkalic system |
| CN106216710A (en) * | 2016-09-29 | 2016-12-14 | 西北有色金属研究院 | A kind of preparation method of high-tap density high-crystallinity silver powder |
| CN107096927A (en) * | 2017-06-13 | 2017-08-29 | 浙江纺织服装职业技术学院 | It is a kind of to reduce the silver powder preparation method of silver powder burn out rate |
| CN107186218A (en) * | 2017-04-18 | 2017-09-22 | 王芳 | A kind of preparation method of modified superfine noble metal powder |
| CN108480616A (en) * | 2018-03-21 | 2018-09-04 | 苏州思美特表面材料科技有限公司 | A kind of powder preparation method of effective control metal powder particles surface roughness |
| CN108714700A (en) * | 2018-06-07 | 2018-10-30 | 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 highly crystalline type silver powder of monodisperse and its silver powder obtained |
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| CN110102777A (en) * | 2019-06-04 | 2019-08-09 | 刘焕明 | A kind of preparation method of the highly crystalline silver powder of induced growth |
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| CN107096927A (en) * | 2017-06-13 | 2017-08-29 | 浙江纺织服装职业技术学院 | It is a kind of to reduce the silver powder preparation method of silver powder burn out rate |
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| CN108714700A (en) * | 2018-06-07 | 2018-10-30 | 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 highly crystalline type silver powder of monodisperse and its silver powder obtained |
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| CN113953523B (en) * | 2021-10-12 | 2023-09-22 | 善日(嘉善)能源科技有限公司 | Preparation method of polyhedral submicron silver powder |
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