A kind of preparation method of highly crystalline flaky silver powder

A flake silver powder and high crystallization technology, applied in the field of preparation of high crystal flake silver powder, can solve the problems of high cost of preparation process, long ball milling time, reduced purity of silver powder, etc., and achieves narrow particle size dispersion range and high tap density. , smooth surface effect

Inactive Publication Date: 2015-12-02
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the application publication number: CN102794453A, the ball milling time is long in the preparation process, and a large amount of additives are introduced in the ball milling process to reduce the purity of the silver powder, and the preparation process consumes a lot of electric energy.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] After cleaning, the reactor and the liquid distribution tank were washed and dried with deionized water. Prepare precursor solution, use diethylene glycol as solvent, including silver nitrate 0.8g / L palladium nitrate 20mg / L; prepare silver ammonia solution, use diethylene glycol as solvent, including silver nitrate 30g / L, ammonia water 100g / L ; Prepare mixed reducing solution, hydrogen peroxide 68.5g, PEG-200002g, ammonia water 20g are mixed with diethylene glycol to prepare mixed reducing solution. While stirring and mixing the reducing solution at high speed, uniformly mix the precursor solution and the mixed reducing solution for reaction, control the reaction temperature at 50° C., and the reaction time for 10 minutes. Continue to stir after the reaction is complete, and add the silver ammonia solution dropwise to it within 30 minutes. After settling for 50 minutes, the supernatant reaction liquid was poured out to collect its precipitate. After settling for 45 mi...

Embodiment 2

[0022] After cleaning, the reactor and the liquid distribution tank were washed and dried with deionized water. Prepare precursor solution, use diethylene glycol as solvent, wherein silver nitrate 2g / L palladium nitrate 14mg / L; prepare silver ammonia solution, use diethylene glycol as solvent, wherein silver nitrate 20g / L, ammonia water 130g / L; Prepare mixed reducing solution, hydrogen peroxide 100g, PEG-200001.5g, ammonia water 45g are mixed with diethylene glycol to prepare mixed reducing solution. While stirring and mixing the reducing solution at high speed, uniformly mix the precursor solution and the mixed reducing solution for reaction, control the reaction temperature at 30° C., and the reaction time for 30 minutes. Continue to stir after the reaction is complete, and add the silver ammonia solution dropwise to it within 45min. After settling for 60 minutes, the supernatant reaction liquid was poured out to collect its precipitate. After settling for 65 minutes, the ...

Embodiment 3

[0024] After cleaning, the reactor and the liquid distribution tank were washed and dried with deionized water. Prepare precursor solution, use diethylene glycol as solvent, including silver nitrate 2.5g / L palladium nitrate 50mg / L; prepare silver ammonia solution, use diethylene glycol as solvent, including silver nitrate 18g / L, ammonia water 80g / L ; Prepare mixed reducing solution, hydrogen peroxide 80g, PEG-200000.5g, ammonia water 15g are mixed with diethylene glycol to prepare mixed reducing solution. While stirring and mixing the reducing solution at high speed, uniformly mix the precursor solution and the mixed reducing solution for reaction, control the reaction temperature at 25° C., and the reaction time for 15 minutes. Continue to stir after the reaction is complete, and add the silver ammonia solution dropwise to it within 20 minutes. After settling for 60 minutes, the supernatant reaction liquid was poured out to collect its precipitate. After settling for 90 min...

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Abstract

The invention relates to a preparation method for high-crystallized flake silver powders. The preparation method includes: adding a polymeric precursor solution to a reduction solution taking diethylene glycol as a solvent and containing PEG-20000 and hydrogen peroxide for hybrid reaction, wherein silver nitrate and trace palladium nitrate are taken as additives, and the polymeric precursor solution is composed by the solvent of the diethylene glycol; continuously adding dropwise a silver ammonia solution taking the diethylene glycol as the solvent into the polymeric precursor solution till reaction is complete, wherein obtained sediment is cleaned and dried to form the high-crystallized flake silver powders. Compared with those by the prior art, the silver powders prepared by the preparation method have the advantages of high tap density, narrow particle-size dispersion scope, smooth surface, low oil adsorption and the like.

Description

technical field [0001] The invention relates to the field of electronic equipment preparation, in particular to electronic paste silver powder and its method in the technical field of solar cells, in particular to a preparation method of highly crystalline flake silver powder. Background technique [0002] As precious metal pastes are widely used in the packaging process of hybrid microcircuits, the performance of precious metal powders has received increasing attention. Among them, ultra-fine silver powders, which are important conductive functional materials for conductors, resistors, and dielectric electronic pastes, are in constant demand. Increase, and the requirements for the performance of metallic silver powder such as particle size and distribution, morphology, specific surface area, etc. are becoming increasingly stringent. At present, the shapes of silver powder are roughly spherical, scaly, dendritic and flake. When flake silver powder is used as a filler to con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
Inventor 胡晓斌宗志杰郑铙
Owner SHANGHAI JIAOTONG UNIV
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