CN114713838A - Preparation method of high-tap small-particle-size sphere-like silver powder for LTCC inner electrode - Google Patents
Preparation method of high-tap small-particle-size sphere-like silver powder for LTCC inner electrode Download PDFInfo
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- CN114713838A CN114713838A CN202210437467.7A CN202210437467A CN114713838A CN 114713838 A CN114713838 A CN 114713838A CN 202210437467 A CN202210437467 A CN 202210437467A CN 114713838 A CN114713838 A CN 114713838A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The invention relates to a preparation method of high-tap small-particle-size sphere-like silver powder for an LTCC inner electrode, which comprises the following steps of: dissolving silver nitrate in pure water to obtain a silver nitrate solution with the concentration of 250-300 g/L; dissolving a reducing agent in pure water to obtain a reducing agent solution with the concentration of 100-180 g/L; dissolving the dispersing agent and the granularity control agent in pure water to obtain a base solution; fourthly, adding a silver nitrate solution and a reducing agent solution into the base solution in a concurrent flow manner, stirring, reacting for 15-20 min, and adding a surface modifier solution to obtain silver powder; fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain an Ag powder filter cake; sixthly, drying the Ag powder filter cake, grinding and screeningThe obtained product has an average particle diameter of 1.0 to 4.0 μm and a tap density of 6.0 to 6.5g/cm3The high-tap small-particle size sphere-like superfine silver powder. The invention uses a liquid phase reduction method to scientifically and reasonably control a reducing agent, a dispersing agent, a granularity control agent and the like in the reduction process, thereby obtaining the superfine silver powder with small granularity and high tap density.
Description
Technical Field
The invention relates to the technical field of precious metal material preparation, in particular to a preparation method of high-tap small-particle-size sphere-like silver powder for an LTCC inner electrode.
Background
With the rapid development of the technical fields of electronic industry, new energy and the like, the ultrafine silver powder is used as a functional material with very high surface activity and excellent electrical conductivity, and is widely applied to the fields of conductive paste, energy industry, composite materials, catalysts, antibacterial materials and the like. The conductive paste is widely applied to the production of various electronic components, such as LTCC, chip components and the like, as a functional material. Silver powder is the most important raw material of the conductive paste, has important influence on parameters such as film forming property, film thickness, electrical property, weldability and adhesiveness in the preparation process, and the quality of the silver powder directly influences the conductive paste and the performance of a finally formed conductor.
At present, a plurality of methods for preparing silver powder at home and abroad mainly comprise a grinding method, an atomization method, an evaporation and condensation method, an electrochemical deposition method, a sol-gel method, a liquid phase reduction method and the like. The liquid phase reduction method has the advantages of simple operation process, low investment, high yield, low loss and good performance, and is one of the most promising preparation methods at present. However, the liquid phase chemical reduction method has the problems of excessively wide silver powder particle size distribution, high organic impurity content, easy formation of agglomerated large particles, difficult sedimentation, difficult solid-liquid separation process, low yield and the like which need to be solved urgently when the silver powder is prepared.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of high-tap small-granularity sphere-like silver powder with high crystallinity and uniform granularity for an LTCC inner electrode.
In order to solve the problems, the preparation method of the high-tap small-particle-size sphere-like silver powder for the LTCC inner electrode comprises the following steps of:
dissolving silver nitrate in pure water to obtain a silver nitrate solution with the concentration of 250-300 g/L, and keeping the temperature to 25-30 ℃;
dissolving a reducing agent in pure water to obtain a reducing agent solution with the concentration of 100-180 g/L, and keeping the temperature to 25-30 ℃;
dissolving a dispersing agent and a granularity control agent in pure water to obtain a base solution, and keeping the temperature to 25-30 ℃;
fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a concurrent flow manner, stirring, reacting for 15-20 min, and adding a surface modifier solution with the concentration of 16-32 g/L to obtain silver powder;
fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain an Ag powder filter cake;
sixthly, drying, grinding and screening the Ag powder filter cake to obtain the Ag powder filter cake with the average particle size of 1.0-4.0 mu m and the tap density of 6.0-6.5 g/cm3The high-tap small-particle size sphere-like superfine silver powder.
The reducing agent is any one of glucose, hydroquinone and hydrazine hydrate.
The addition amount of the dispersing agent in the middle base solution is 100-200 g/L, and the addition amount of the granularity control agent is 0.27-5.0 g/L; the dispersing agent is one of lactic acid, polyvinylpyrrolidone and gelatin; the granularity control agent is ammonia water with the concentration of 25%.
The cocurrent stirring condition in the step four is that the speed of cocurrent adding of the silver nitrate solution and the reducing agent solution into the base solution is 67-100 mL/min, the liquid adding time is 10-15 min, the stirring rotating speed is 400-600 rpm, and the reaction time is 15-20 min.
The surface modifier solution with the concentration of 16-32 g/L in the step four is a solution obtained by dissolving a surface modifier in an absolute ethyl alcohol solution; the surface modifier is one of stearic acid, erucic acid and polyacrylamide, and the addition amount of the surface modifier is 0.5-1.0% of the theoretical content of the silver powder.
The drying condition in the step sixteenth means that the temperature is 65-75 ℃ and the time is 15-20 hours.
Compared with the prior art, the invention has the following advantages:
1. the silver powder is prepared by adding a reducing agent solution and a metal salt solution into a dispersant solution in a cocurrent manner, controlling the temperature and the liquid adding speed of a reaction system and assisting with a particle size control agent; the purpose of obtaining the silver powder product with high crystallinity and uniform granularity is achieved by controlling the nucleation and the growth rate of the silver powder.
2. The dispersant added in the invention is to ensure that no dispersant remains after the silver powder is washed and dried.
3. According to the invention, the surface of the silver powder particles can be coated by adding the surfactant after the silver powder particles are subjected to parallel flow, so that the modification effect is achieved, the agglomeration in the subsequent washing and drying processes is prevented, and the dispersibility and tap density of the synthesized silver powder are improved.
4. The invention uses a liquid phase reduction method to scientifically and reasonably control a reducing agent, a dispersing agent, a granularity control agent and the like in the reduction process, thereby obtaining the superfine silver powder with small granularity and high tap density.
5. The method has the advantages of simple operation, wide raw material source, low cost, low requirement on equipment and easy realization of industrial production.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is an SEM photograph of the ultrafine silver powder of example 1 of the present invention.
FIG. 3 is an SEM photograph of the ultrafine silver powder of example 2 of the present invention.
FIG. 4 is an electron micrograph of the ultrafine silver powder according to example 3 of the present invention.
Detailed Description
As shown in fig. 1, a method for preparing high-tap small-particle-size spheroidal silver powder for an LTCC inner electrode comprises the following steps:
dissolving silver nitrate in pure water to obtain a silver nitrate solution with the concentration of 250-300 g/L, and keeping the temperature to 25-30 ℃.
Dissolving a reducing agent in pure water to obtain a reducing agent solution with the concentration of 100-180 g/L, and keeping the temperature to 25-30 ℃; the reducing agent is any one of glucose, hydroquinone and hydrazine hydrate.
Dissolving a dispersing agent and a granularity control agent in pure water to obtain a base solution, and keeping the temperature to 25-30 ℃; the addition amount of the dispersing agent in the base solution is 100-200 g/L, and the addition amount of the granularity control agent is 0.27-5.0 g/L; the dispersant is one of lactic acid, polyvinylpyrrolidone and gelatin; the granularity control agent is ammonia water with the concentration of 25 percent.
And fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, wherein the parallel flow liquid adding speed is 67-100 mL/min, the liquid adding time is 10-15 min, and the stirring rotating speed is 400-600 rpm. And (3) reacting for 15-20 min, and adding a surface modifier solution with the concentration of 16-32 g/L to obtain the silver powder.
Wherein: the surface modifier solution with the concentration of 16-32 g/L is a solution obtained by dissolving a surface modifier in an absolute ethyl alcohol solution; the surface modifier is one of stearic acid, erucic acid and polyacrylamide, and the addition amount of the surface modifier is 0.5-1.0% of the theoretical content of the silver powder.
Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain the Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 65-75 ℃ for 15-20 h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 1.0-4.0 mu m and the tap density of 6.0-6.5 g/cm3The high-tap small-particle size sphere-like superfine silver powder.
Embodiment 1 a method for preparing high tap density small particle size spheroidal silver powder for LTCC internal electrodes, comprising the steps of:
firstly, dissolving 250g of silver nitrate in 1L of pure water to obtain a silver nitrate solution, and keeping the temperature to 25 ℃.
Dissolving 180g of glucose in 1L of pure water to obtain a reducing agent solution, and keeping the temperature to 25 ℃.
Dissolving 200g of polyvinylpyrrolidone and 1.8g of ammonia water in 1L of pure water to obtain a base solution, and keeping the temperature to 25 ℃.
And fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, adding liquid at a speed of 67mL/min in a parallel flow manner for 15min, stirring at a rotating speed of 600rpm, reacting for 15min, and adding the surface modifier solution to obtain the silver powder.
Wherein: the surface modifier solution is a solution of 0.8g polyacrylamide in 0.05L absolute ethanol. Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain the Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 75 ℃ for 16h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 1.25 mu m and the tap density of 6.0g/cm3The high-tap small-particle size sphere-like superfine silver powder.
The obtained ultrafine silver powder was subjected to electron microscope scanning, as shown in FIG. 1. As can be seen from the figure, the silver powder has uniform particle size, small particle size, good dispersibility and agglomeration.
Embodiment 2 a method for preparing high tap density small particle size spheroidal silver powder for LTCC internal electrodes, comprising the steps of:
dissolving 250g of silver nitrate in 1L of pure water to obtain a silver nitrate solution, and keeping the temperature constant to 30 ℃.
Dissolving 180g of glucose in 1L of pure water to obtain a reducing agent solution, and keeping the temperature to 30 ℃.
Dissolving 200g of polyvinylpyrrolidone and 1.0g of ammonia water in 1L of pure water to obtain a base solution, and keeping the temperature to 30 ℃.
Fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, wherein the parallel flow liquid adding speed is 100mL/min, the liquid adding time is 10min, and the stirring rotating speed is 600 rpm. And adding a surface modifier solution after reacting for 20min to obtain the silver powder.
Wherein: the surface modifier solution was the same as in example 1.
Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain the Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 75 ℃ for 16h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 1.48 mu m and the tap density of 6.2g/cm3The high-tap small-particle size sphere-like superfine silver powder.
The obtained ultrafine silver powder was subjected to electron microscope scanning, as shown in FIG. 2. As can be seen from the figure, the silver powder particles were uniform in size, small in size, better in dispersibility than that of example 1, and had a small amount of agglomerates.
Embodiment 3 a method for preparing high tap density small particle size spheroidal silver powder for LTCC internal electrodes, comprising the steps of:
firstly, dissolving 250g of silver nitrate in 1L of pure water to obtain a silver nitrate solution, and keeping the temperature to 25 ℃.
Dissolving 180g of glucose in 1L of pure water to obtain a reducing agent solution, and keeping the temperature to 25 ℃.
Dissolving 200g of polyvinylpyrrolidone and 0.27g of ammonia water in 1L of pure water to obtain a base solution, and keeping the temperature to 25 ℃.
Fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, wherein the parallel flow liquid adding speed is 70mL/min, the liquid adding time is 14min, and the stirring rotating speed is 400 rpm. And adding a surface modifier solution after reacting for 20min to obtain the silver powder.
Wherein: the surface modifier solution was the same as in example 1.
Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, carrying out solid-liquid separation, and obtaining an Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 75 ℃ for 16h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 1.42 mu m and the tap density of 6.3g/cm3The high-tap small-particle size sphere-like superfine silver powder.
The obtained ultrafine silver powder was subjected to electron microscope scanning, as shown in FIG. 3. As can be seen from the figure, the silver powder has uniform particle size, small particle size, good dispersibility and no agglomeration.
Embodiment 4 a method for preparing high tap density small particle size spheroidal silver powder for LTCC internal electrodes, comprising the steps of:
firstly, dissolving 250g of silver nitrate in 1L of pure water to obtain a silver nitrate solution, and keeping the temperature to 25 ℃.
Dissolving 100g of hydroquinone in 1L of pure water to obtain a reducing agent solution, and keeping the temperature to 25 ℃.
Dissolving 100g of gelatin dispersant and 1.0g of ammonia water in 1L of pure water to obtain a base solution, and keeping the temperature to 25 ℃.
Fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, wherein the parallel flow liquid adding speed is 100mL/min, the liquid adding time is 10min, and the stirring rotating speed is 500 rmp. And adding a surface modifier solution after reacting for 15min to obtain the silver powder.
Wherein: the surface modifier solution is a solution of 1.58g of stearic acid in 0.05L of absolute ethanol.
Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain the Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 75 ℃ for 16h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 1.45 mu m and the tap density of 6.15g/cm3The high-tap small-particle size sphere-like superfine silver powder.
Embodiment 5 a method for preparing high tap density small particle size spheroidal silver powder for LTCC internal electrodes, comprising the steps of:
dissolving 250g of silver nitrate in 1L of pure water to obtain a silver nitrate solution, and keeping the temperature constant to 30 ℃.
Dissolving 150g of hydrazine hydrate in 1L of pure water to obtain a reducing agent solution, and keeping the temperature to 30 ℃.
Thirdly, dissolving 150g of lactic acid and 5.0g of ammonia water in 1L of pure water to obtain a base solution, and keeping the temperature to 30 ℃.
Fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a parallel flow manner for stirring, wherein the parallel flow liquid adding speed is 100mL/min, the liquid adding time is 10min, and the stirring rotating speed is 500 rmp. And adding a surface modifier solution after reacting for 15min to obtain the silver powder.
Wherein: the surface modifier solution is a solution of 1.0g of erucic acid dissolved in 0.05L of absolute ethanol.
Fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain the Ag powder filter cake.
Sixthly, drying the Ag powder filter cake at 75 ℃ for 16h, grinding and screening to obtain the Ag powder filter cake with the average particle size of 3.45 mu m and the tap density of 6.0g/cm3The high-tap small-particle size sphere-like superfine silver powder.
Claims (6)
1. A preparation method of high-tap small-particle-size sphere-like silver powder for an LTCC inner electrode comprises the following steps:
dissolving silver nitrate in pure water to obtain a silver nitrate solution with the concentration of 250-300 g/L, and keeping the temperature to 25-30 ℃;
dissolving a reducing agent in pure water to obtain a reducing agent solution with the concentration of 100-180 g/L, and keeping the temperature to 25-30 ℃;
dissolving a dispersing agent and a granularity control agent in pure water to obtain a base solution, and keeping the temperature to 25-30 ℃;
fourthly, adding the silver nitrate solution and the reducing agent solution into the base solution in a concurrent flow manner, stirring, reacting for 15-20 min, and adding a surface modifier solution with the concentration of 16-32 g/L to obtain silver powder;
fifthly, washing the silver powder until the conductivity of the washing liquor is less than or equal to 20 microseconds, and carrying out solid-liquid separation to obtain an Ag powder filter cake;
sixthly, drying, pulverizing and screening the Ag powder filter cake to obtain the Ag powder filter cake with the average particle size of 1.0-4.0 mu m and the tap density of 6.0-6.5 g/cm3The high-tap small-particle size sphere-like superfine silver powder.
2. The method of making high tap small particle size spheroidal silver powder for LTCC internal electrodes of claim 1, wherein: the reducing agent is any one of glucose, hydroquinone and hydrazine hydrate.
3. The method of making high tap small particle size spheroidal silver powder for LTCC internal electrodes of claim 1, wherein: the addition amount of the dispersing agent in the middle base solution is 100-200 g/L, and the addition amount of the granularity control agent is 0.27-5.0 g/L; the dispersing agent is one of lactic acid, polyvinylpyrrolidone and gelatin; the granularity control agent is ammonia water with the concentration of 25%.
4. The method of making high tap small particle size spheroidal silver powder for LTCC internal electrodes of claim 1, wherein: the cocurrent stirring condition in the step four is that the speed of cocurrent adding of the silver nitrate solution and the reducing agent solution into the base solution is 67-100 mL/min, the liquid adding time is 10-15 min, the stirring rotating speed is 400-600 rpm, and the reaction time is 15-20 min.
5. The method for preparing high-tap small-particle-size spheroidal silver powder for an LTCC inner electrode as claimed in claim 1, wherein the method comprises the following steps: the surface modifier solution with the concentration of 16-32 g/L in the step four is a solution obtained by dissolving a surface modifier in an absolute ethyl alcohol solution; the surface modifier is one of stearic acid, erucic acid and polyacrylamide, and the addition amount of the surface modifier is 0.5-1.0% of the theoretical content of the silver powder.
6. The method of making high tap small particle size spheroidal silver powder for LTCC internal electrodes of claim 1, wherein: the drying condition in the step sixteenth means that the temperature is 65-75 ℃ and the time is 15-20 hours.
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| CN116809945A (en) * | 2023-05-11 | 2023-09-29 | 湖北银科新材料股份有限公司 | Spherical silver powder and preparation method thereof |
| CN117300145A (en) * | 2023-09-21 | 2023-12-29 | 上海银波生物科技有限公司 | Preparation method of monocrystal-like silver powder with ultrahigh tap density |
| CN117600480A (en) * | 2023-11-30 | 2024-02-27 | 广西建兴光银新材料科技有限公司 | Spherical superfine silver powder and preparation method and application thereof |
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