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Preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size

A monodisperse, high crystallization technology, applied in the field of electronic components, can solve the problems of unsuitable high resolution and single particle size of silver powder, and achieve the effect of narrow particle size dispersion range, smooth surface and high sphericity

Inactive Publication Date: 2012-07-11
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of the output silver powder is single, which is not suitable for the preparation of silver paste with high resolution and high conductivity.

Method used

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  • Preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size
  • Preparation method of mono-dispersed highly crystalline silver powder with adjustable particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] For the reaction vessel, stirring blade, etc., at 85℃, Na 3 PO 4 95g / L, Na 2 CO 3 120g / L, NaOH130g / L, H 2 O 2 Wash in a 25ml / L solution for 15 minutes, and then wash with deionized water.

[0021] Prepare acidic silver salt solution with 0.30mol / L of silver nitrate. Prepare mixed reducing solution. L-ascorbic acid 0.16mol / L, PVP 0.009mol / L, potassium nitrate 0.60g / L are prepared into a mixed reducing solution with deionized water. Finally, adjust the pH of the mixed reducing solution to 1. While stirring and mixing the reducing solution at a low speed, quickly mix the acidic silver salt solution and the mixed reducing solution uniformly for reaction, and control the reaction temperature at 20° C. and the reaction time for 8 minutes. Post-treatment of the silver powder after the reaction. After settling for 2 hours anyway, the supernatant reaction solution was poured out, and then the precipitated silver powder was washed with deionized water to a conductivity of 20 μ...

Embodiment 2

[0024] For the reaction vessel, stirring blade, etc., at 90℃, Na 3 PO 4 98g / L, Na 2 CO 3 130g / L, NaOH140g / L, H 2 O 2 Rinse in 20ml / L solution for 20min, then rinse with deionized water.

[0025] Prepare acidic silver salt solution with 0.40mol / L silver nitrate. Prepare mixed reducing solution. L-ascorbic acid 0.22mol / L, oleic acid 0.02mol / L, potassium carbonate 0.35g / L are prepared with deionized water to prepare a mixed reducing solution. Finally, adjust the pH of the mixed reducing solution to 0.3. While stirring and mixing the reducing solution at low speed, quickly mix the acidic silver salt solution and the mixed reducing solution uniformly for reaction, and control the reaction temperature at 25° C. and the reaction time for 6 min. Post-treatment of the silver powder after the reaction. After settling for 3 hours anyway, the supernatant reaction solution was poured out, and then the precipitated silver powder was washed with deionized water to a conductivity of 35 μs / ...

Embodiment 3

[0028] For the reaction vessel, stirring blade, etc., at 80℃, Na 3 PO 4 100g / L, Na 2 CO 3 130g / L, NaOH150g / L, H 2 O 2 Wash in a 25ml / L solution for 15 minutes, and then wash with deionized water.

[0029] Prepare acidic silver salt solution with 0.35mol / L of silver nitrate. Prepare mixed reducing solution. L-ascorbic acid 0.18mol / L, ammonium stearate 0.025mol / L, potassium sulfate 0.8g / L are prepared with deionized water to prepare a mixed reducing solution. Finally, adjust the pH of the mixed reducing solution to 0.5. While stirring and mixing the reducing solution at low speed, quickly mix the acidic silver salt solution and the mixed reducing solution uniformly for reaction, and control the reaction temperature at 30°C and the reaction time for 10 minutes. Post-treatment of the silver powder after the reaction. After settling for 4 hours anyway, the supernatant reaction solution was poured out, and then the precipitated silver powder was washed with deionized water to a c...

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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 [0001] The invention relates to a material and a method in the field of electronic components, in particular to a preparation method of monodisperse high crystalline silver powder with adjustable particle size. Background technique [0002] The preparation of high-purity, high-dispersion, and ultra-fine powders is one of the current hot spots in materials 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 electronic technology, the precision and miniaturization of printed circuits and electronic components, silver powder is required to develop in the direction of high purity, high dispersion and ultrafineness, and the shape of the silver powder is as spherical or quasi-spherical as possible. [0003] The preparation methods of silver powder include gas phase method, solid phase method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 胡晓斌宗志杰李浩然钱宇伟赵斌元
Owner SHANGHAI JIAO TONG UNIV
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