CN1227148A - High purity high dispersiveness spherical super fine silver powder and its producing method - Google Patents
High purity high dispersiveness spherical super fine silver powder and its producing method Download PDFInfo
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- CN1227148A CN1227148A CN 99112631 CN99112631A CN1227148A CN 1227148 A CN1227148 A CN 1227148A CN 99112631 CN99112631 CN 99112631 CN 99112631 A CN99112631 A CN 99112631A CN 1227148 A CN1227148 A CN 1227148A
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Abstract
The superfine powder is produced by using silver ingot as material and through the process of the dissolution of silver ingot with nitric acid to produce silver nitrate solution, the reduction with formate to produce silver powder, the dissolution of silver powder with nitric acid to produce high-purity silver nitrate solution, the mixing of the high-purity silver nitrate solution with dispersant and ammonia water to produce complex silver-ammonia ion solution, the mixing of the complex ion solution with reducer solution in special nozzle while stirring with high-capacity stirrer to produce high dispersiveness spherical superfine silver powder. The present invention can control the final purity of the silver powder effectively through the control of the purity of silver nitrate solution and may be used in industrial production.
Description
The invention relates to a method for preparing silver powder by a chemical method, in particular to a method for preparing high-purity high-dispersity spherical superfine silver powder by a reduction method and a production method thereof.
The preparation of high-purity, high-dispersion and ultrafine powder is one of the hot spots of the current material science research. In the electronics industry, silver powder is widely used in the manufacture of various conductive pastes for printed circuits and internal and external electrodes of electronic components. Due to the development of microelectronics, the precision and miniaturization of printed circuits and electronic components, silver powders are required to be developed in the direction of high purity, high dispersion and ultra-fine, and to be as spherical or spheroidal in shape as possible.
Silver powder can be produced by chemical, physical and electrochemical methods. Silver powders used in the electronics industry are typically produced by chemical reduction, i.e., by reacting a soluble silver salt with a suitable reducing agent under conditions to produce a silver powder. The reducing agents commonly used include hydrazine, formate, sulfite, hypophosphite, saccharides and aldehydes.
There are many patents applying for silver powder at home and abroad, but the patents do not describe the purity control of the silver powder, and the dispersibility of the silver powder is only started by selecting various dispersants, is not controlled from a reaction process, and cannot be amplified to an industrialized process. The chemical precipitation process comprises two processes of reaction nucleation and crystal nucleus growth, and because the reaction nucleation process is a rapid instant reaction (millisecond level), the reactants must be instantly uniform at a molecular level in a reactor, namely micro-mixing is realized, and the product forms can be consistent as much as possible.
The invention aims to provide a method for industrially producing high-purity high-dispersity spherical superfine silver powder by controlling a reaction process and a production method thereof.
The object of the invention is achieved in that:
the silver ingot is prepared by using commercial industrial-grade silver ingot with purity of more than 90% as a raw material, dissolving the commercial industrial-grade silver ingot by nitric acid to prepare a silver nitrate solution, adding alkaline reagents which are alkali metal hydroxide or carbonate, adjusting the pH value of the solution, controlling the pH value to be between 5.5 and 6.5, preferably between 5.7 and 6.0, adding formate (namely sodium formate and ammonium formate), filtering suspension, using the formate as a reducing agent, dissolving the obtained silver powder by nitric acid to prepare a high-purity silver nitrate solution, wherein the concentration of the silver nitrate solution is between 0.12 and 2.4M, mixing the high-purity silver nitrate solution with a dispersing agent, wherein the dispersing agent can be commercial polyethylene pyrrolidone and gelatin, and can also be alcohol amine compounds such as monoethanolamine, diethanolamine and triethanolamine, adding ammonia water to prepare a silver ammonia complex ion solution, and adjusting the pH to be between 10 and 12; it is mixed with the reducing agent such as: formaldehyde, hydrazine and hydroquinone are prepared into a reducing agent solution, the pH = 9-11 in the reaction process is controlled, the reaction temperature is 10-90 ℃, the reducing agent solution is mixed through a special spray head, a high-energy stirrer is used for stirring, high-dispersity spherical superfine silver powder is prepared, the prepared high-dispersity spherical superfine silver powder is washed and filtered by deionized water until the conductivity of filtrate is less than 20 microohm, the filtrate is washed by ethanol or acetone for one or two times, and a finished product is prepared after drying.
The invention has the advantages that: the reaction process is effectively controlled, so that industrial production can be carried out; the final purity of the silver powder can be controlled by controlling the purity of the silver nitrate solution; the reaction can be kept consistent in reaction systems of different scales through a special spray head; and a high-energy stirrer is matched with the dispersing agent to control the high dispersibility of the silver powder.
The silver powder is spherical or quasi-spherical, the total content of impurities is not more than 100ppm, the thermal weight loss at 1000 ℃ is not more than 2.0 percent, and the specific surface area is 0.6-2.0 m2(g), particle size distribution range of 0.1-3 μm, tap density of 3.0-4.5 g/dm2。
The production of the ultra-pure high-dispersibility spherical ultrafine silver powder comprises the following steps (see fig. 2):
1 preparing a high-purity silver nitrate solution from silver ingots; the preparation method of the high-purity silver nitrate solution comprises the following steps:
1.1 dissolving silver ingots in an analytically pure nitric acid solution to prepare a silver nitrate solution;
1.2 adding an alkaline reagent with analytical purity into a silver nitrate solution to precipitate insoluble metal impurities;
1.3 adding a reducing agent into relatively pure silver nitrate solution to precipitate silver powder, and leaving impurities in the reaction solution;
1.4, cleaning the precipitated silver powder, and dissolving the silver powder in an analytically pure nitric acid solution to prepare a high-purity silver nitrate solution.
The silver ingot used in the present invention is an industrial grade silver ingot with a purity of 90% or more on the market.
Silver ingots were dissolved in an analytically purenitric acid solution and the reaction system was slowly heated to 90 ℃ for complete dissolution. The dissolution reaction can be expressed by the following equation:
adding an alkaline reagent into the silver nitrate solution to precipitate insoluble metal impurities to prepare relatively pure silver nitrate solution. The alkaline agent which can be used includes hydroxides and carbonates of alkali metals such as sodium hydroxide, potassium hydroxide, lithium hydroxide and sodium carbonate. Sodium hydroxide is preferred from the viewpoint of cost and efficiency. In the neutralization reaction process, the pH of the solution is controlled to be 5.5-6.5. Too high a pH causes precipitation of silver oxide, resulting in a decrease in the yield of the final product, and too low a pH causes a decrease in the efficiency of removing impurities. The filtering process can remove most of base metal impurities such as iron, copper, lead, zinc and the like and a small amount of non-metal impurities such as arsenic, selenium, antimony, phosphorus, sulfur, boron, halogen and the like.
After the precipitation reaction, impurities can be separated from the relatively pure silver nitrate solution by centrifugation or filtration. The obtained silver nitrate solution still contains alkali metal, alkaline earth metal, and a small amount of base metal and non-metallic impurities such as arsenic, selenium, antimony and the like which are not completely precipitated.
The next step is to add a "selective reducing agent" to the relatively pure silver nitrate solution, where the "selective reducing agent" is a reducing agent that reduces silver ions to silver powder without reducing other impurities to a metallic state. Formate such as sodium formate, ammonium formate are the most effective reducing agent, especially sodium formate, use it as reducing agent have cost low, easy to operate, reaction rate fast, silver powder particle size advantage such as being easy to control.
The reaction of silver nitrate solution with sodium formate is:
in order to complete the reduction reaction, the amount of sodium formate is 10-20% more than the theoretical value.
The precipitation reaction greatly improves the purity of the silver powder, all impurities are left in the reaction solution, and the silver powder is separated by using a proper solid-liquid separation method such as centrifugation, filtration and the like and is washed by using deionized water. And finally, dissolving the pure silver powder by using an analytically pure nitric acid solution to obtain a high-purity silver nitrate solution.
2, preparing the high-dispersity spherical ultrafine silver powder from the high-purity silver nitrate solution comprises the following steps:
2.1 mixing a high-purity silver nitrate solution with a dispersing agent, adding ammonia water to prepare a silver-ammonia complex ion solution, and adjusting the pH = 10-12;
2.2 dissolving a reducing agent in deionized water to prepare a reducing agent solution;
2.3, mixing the reducing agent solution and the silver-ammonia complex ion solution through a special spray head, and stirring and mixing the mixture by using a high-energy stirrer, wherein the pH = 9-11 in the reaction process and the reaction temperature is controlled to be 10-90 ℃;
2.4 washing the silver powder by deionized water, and filtering until the conductivity of the filtrate is less than 20 microohm. Cleaning with ethanol or acetone for one or two times, and drying to obtain the final product.
The concentration of the high-purity silver nitrate solution is controlled to be between 0.12 and 2.4M, the production efficiency is reduced when the concentration is too low, the granularity of the silver powder is increased when the concentration is too high, and the best concentration is controlled to be between 0.3 and 1.2M.
The dispersant used may be chosen from a wide variety of commercially available polyvinylpyrrolidones, gelatins, and also ethanolamines such as monoethanolamine, diethanolamine, triethanolamine. The ratio of the dispersing agent to the silver ions is 0-0.2: 1 (molar ratio).
Adding ammonia water into a mixed solution of a high-purity silver nitrate solution and a dispersing agent to prepare a silver-ammonia complex ion solution, and controlling the pH = 10-12 of the solution.
The reducing agent of the present invention may be selected from a variety of materials, and preferably formaldehyde, hydrazine or hydroquinone is used. In order to complete the reduction reaction, the reducing agent should be 10-30% more than the theoretical value.
The silver-ammonia complex ion solution and the reducing agent are mixed in a double-flow external mixing type spray head through pipelines respectively, a high-shear type stirrer is used for stirring, the PH = 9-11 in the reaction process is controlled, and the reaction temperature is 10-90 ℃.
And washing the precipitated silver powder by using deionized water, and filtering until the conductivity of the filtrate is less than 20 microohm. Cleaning with ethanol or acetone for one or two times, and drying to obtain thefinal product.
The production process of the present invention will be further described with reference to examples.
Example 1 in a container with a volume of 120L, 52.68Kg of silver ingot with a purity of 95% and 58L of analytically pure nitric acid solution were added, and the reaction system was heated to 50-90 ℃ until the silver ingot was completely dissolved. A 20% sodium hydroxide solution was added with stirring to adjust the PH of the solution =5.8, and the suspension was filtered to separate the precipitate from the solution. The filtrate was diluted with deionized water to a silver nitrate concentration of 2.5M. 13.96Kg of sodium formate was dissolved in 120L of deionized water. Adding silver nitrate solution into sodium formate solution under stirring, keeping reaction temperature at 50 + -5 deg.C, reacting for 60min, and washing the silver powder with 400L deionized water.
Putting the cleaned silver powder into a 120L container, adding 55L of analytically pure concentrated nitric acid, heating the reaction system to 40-70 ℃ until the silver powder is completely dissolved, continuously heating to 95 ℃ under stirring, keeping the temperature for 2h, removing all nitrogen oxide gas in the solution, and cooling the solution to room temperature to obtain the high-purity silver nitrate solution.
The concentration of the highly pure silver nitrate solution was adjusted to 1.2M with deionized water and an analytically pure aqueous ammonia solution was added with stirring, controlling the solution PH =11.5 ± 0.5 and the temperature 40 ± 2 ℃.
Dissolving 20Kg of hydroquinone in 400L of deionized water, and heating to 40 +/-2 ℃.
Mixing the silver-ammonia complex ion solution and the hydroquinone solution in a spray head shown in figure 1 at the same time, stirring by using a high-shear emulsifying machine, and reacting for 30min, wherein the pH of the system is =10, and the temperature is 50 +/-2 ℃.
And separating the precipitated silver powder from the reaction solution, washing with deionized water until the conductivity of the washing solution is not more than 20 microohm, washing the silver powder twice with ethanol, and drying to obtain 50Kg of finished silver powder.
Example 2 in a container with a volume of 120L, 52.68Kg of silver ingot with a purity of 95% and 58L of analytically pure nitric acid solution were added, and the reaction system was heated to 50-90 ℃ until the silver ingot was completely dissolved. A 20% sodium hydroxide solution was added with stirring to adjust the PH of the solution =5.8, and the suspension was filtered to separate the precipitate from the solution. The filtrate was diluted with deionized water to a silver nitrate concentration of 2.5M. 13.96Kg of ammonium formate were dissolved in 120L of deionized water and the rest was the same as in example 1.
Example 3. the same procedure as in example 1 was repeated except that 2Kg of triethanolamine dispersant was added to the highly pure silver nitrate solution.
Example 4 the same procedure as in example 1 was repeated, except that 85L of formaldehyde and 100L of 20% sodium hydroxide were used as reducing agents.
Example 5, 50L of hydrazine was mixed with 120L of deionized water as a reducing agent, and the rest of the procedure was the same as in example 1.
Example 6 the same procedure as in example 1 was repeated except that 4Kg of polyvinylpyrrolidone dispersant was added to the highly pure silver nitrate solution.
Example 7 the same procedure as in example 1 was repeated except that 2Kg of gelatin dispersant was added to the highly pure silver nitrate solution.
Example 8 the same procedure as in example 1 was repeated except that 2Kg of triethanolamine dispersant was added to the highly pure silver nitrate solution.
Claims (10)
1. A high-purity high-dispersibility spherical superfine silver powder and a production method thereof are characterized in that: dissolving silver ingots serving as raw materials by nitric acid to prepare a silver nitrate solution, adding an alkaline reagent, adjusting the pH value of the solution, adding formate, filtering the suspension, using the formate as a reducing agent, and dissolving the obtained silver powder by nitric acid to prepare a high-purity silver nitrate solution; mixing high-purity silver nitrate solution with a dispersant, adding ammonia water to prepare silver-ammonia complex ion solution, mixing the silver-ammonia complex ion solution with a reducing agent solution through a special spray head, and stirring by using a high-energy stirrer to prepare the high-dispersibility spherical ultrafine silver powder.
2. The method for producing spherical ultrafine silver powder with high purity and high dispersibility according to claim 1, wherein the method comprises the following steps: the formate is sodium formate or ammonium formate.
3. The high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: the silver ingot is commercial industrial grade silver ingot with the purity of more than 90 percent.
4. The method for producing spherical ultrafine silver powder with high purity and high dispersibility according to claim 1, wherein the method comprises the steps of: the alkaline reagent may be an alkali metal hydroxide or carbonate.
5. The high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: the pH value of the neutralization reaction is controlled to be between 5.5 and 6.5, and preferably between 5.7 and 6.0.
6. The high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: adding ammonia water to prepare a silver-ammonia complex ion solution, and adjusting the pH to be 10-12;
7. the high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: mixing a reducing agent solution and a silver-ammonia complex ion solution through a special spray head, and stirring and mixing the reducing agent solution and the silver-ammonia complex ion solution by using a high-energy stirrer, wherein the reducing agent can be formaldehyde, hydrazine and hydroquinone, the pH = 9-11 in the reaction process is controlled, and the reaction temperature is 10-90 ℃;
8. the high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: washing the prepared high-dispersity spherical superfine silver powder with deionized water, filtering until the conductivity of filtrate is less than 20 microohm, washing with ethanol or acetone for one or two times, and drying to obtain a finished product;
9. the high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: the concentration of the silver nitrate solution is 0.12-2.4M.
10. The high-purity high-dispersibility spherical ultrafine silver powder and the production method thereof according to claim 1, wherein the high-purity high-dispersibility spherical ultrafine silver powder comprises: the dispersant can be commercially available polyvinylpyrrolidone and gelatin, and can also be alcohol amine compounds such as monoethanolamine, diethanolamine and triethanolamine.
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| CN 99112631 CN1227148A (en) | 1999-01-19 | 1999-01-19 | High purity high dispersiveness spherical super fine silver powder and its producing method |
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| CN1700360B (en) * | 2004-05-19 | 2010-10-06 | 同和控股（集团）有限公司 | Spherical silver powder and method for producing same |
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| CN102699344A (en) * | 2012-05-18 | 2012-10-03 | 西北稀有金属材料研究院 | Method for preparing micron-scale high-crystallinity spherical silver powder |
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- 1999-01-19 CN CN 99112631 patent/CN1227148A/en active Pending
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| CN1700360B (en) * | 2004-05-19 | 2010-10-06 | 同和控股（集团）有限公司 | Spherical silver powder and method for producing same |
| CN100542719C (en) * | 2004-06-18 | 2009-09-23 | 同和控股（集团）有限公司 | Ball shape silver powder and manufacture method thereof |
| CN102172777A (en) * | 2011-03-04 | 2011-09-07 | 上海交通大学 | High tap density spherical silver powder and preparation and application thereof |
| CN102699344A (en) * | 2012-05-18 | 2012-10-03 | 西北稀有金属材料研究院 | Method for preparing micron-scale high-crystallinity spherical silver powder |
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