Preparation method for micro-order platy silver powder

A flaky silver powder, micron-level technology, applied in the field of preparation of micron-sized flaky silver powder, can solve the problems of not being able to produce particle sizes that meet the requirements, inconsistent technical indicators, and reducing the purity of flaky silver powder, so as to save pollution and High energy consumption, wide reaction temperature range and excellent product quality

Active Publication Date: 2012-10-31
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the ball milling process, there are many variable conditions, resulting in flake silver powders manufactured by different processes, different production cycles or the same production cycle and the same process, which cannot be consistent in terms of technical indicators.
In addition, it is easy to bring in impurities in the ball milling step, reducing the purity of the flake silver powder, and it will also harden, which cannot produce the particle size that meets the requirements, and the energy consumption is high

Method used

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  • Preparation method for micro-order platy silver powder
  • Preparation method for micro-order platy silver powder
  • Preparation method for micro-order platy silver powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of AgNO 3 Aqueous solution: a certain mass of solid AgNO 3 Dissolved in a certain volume of deionized water to prepare AgNO with a mass concentration of 16g / L 3 aqueous solution, and adjust its pH to 3.0 with dilute nitric acid solution;

[0026] (2) Prepare an aqueous solution of reducing agent ascorbic acid: prepare an aqueous solution of ascorbic acid with a mass concentration of 12 g / L;

[0027] (3) Prepare an inducer sulfuric acid aqueous solution with a mass concentration of 180g / L;

[0028] (4) Reduction reaction, liquid-solid separation: 20mL of sulfuric acid aqueous solution with a mass concentration of 180g / L and 200mL of ascorbic acid solution with a mass concentration of 12g / L were mixed into 200mL of silver nitrate solution successively at room temperature 25°C and in a stirring state, and the reaction After 3 minutes, stop the stirring, let stand for 30 minutes, and separate the solid and liquid to obtain a solid product;

[0029] (5) C...

Embodiment 2

[0032] (1) Prepare AgNO with a mass concentration of 40g / L 3 Aqueous solution whose pH is adjusted to 5.0 with dilute nitric acid solution;

[0033] (2) Prepare an aqueous solution of reducing agent ascorbic acid: prepare an aqueous solution of ascorbic acid with a mass concentration of 32 g / L;

[0034] (3) Prepare an inducer sulfuric acid aqueous solution with a mass concentration of 180g / L;

[0035] (4) Reduction reaction, liquid-solid separation: 100mL of sulfuric acid aqueous solution with a mass concentration of 180g / L and 500mL of ascorbic acid solution with a mass concentration of 32g / L were mixed into 500mL of silver nitrate solution successively under stirring at room temperature at 30°C. After 5 minutes, stop the stirring and let stand for 120 minutes; separate the solid and liquid to obtain a solid product;

[0036] (5) Cleaning and drying of the solid product: The solid product obtained in step (4) was washed with deionized water and absolute ethanol until the pH...

Embodiment 3

[0039] (1) Prepare AgNO with a mass concentration of 120g / L 3 Aqueous solution whose pH is adjusted to 3.0 with dilute nitric acid solution;

[0040] (2) Prepare an aqueous solution of reducing agent ascorbic acid: prepare an aqueous solution of ascorbic acid with a mass concentration of 96 g / L;

[0041] (3) Prepare an aqueous solution of inducer sodium sulfate with a mass concentration of 100g / L;

[0042](4) Reduction reaction, liquid-solid separation: 120mL of sodium sulfate aqueous solution with a mass concentration of 100g / L and 400mL of ascorbic acid solution with a mass concentration of 96g / L were mixed into 400mL with a mass concentration of 120g at a room temperature of 35°C and under stirring. / L of silver nitrate solution, after reacting for 3min, stop stirring, and let stand for 80min; solid-liquid separation, to obtain solid product;

[0043] (5) Cleaning and drying of the solid product: The solid product obtained in step (4) was washed with deionized water and a...

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Abstract

The invention discloses a preparation method for a micro-order platy silver powder, which comprises the following steps: preparing 10-180g/L AgNo3 aqueous solution, and regulating the pH value to be 2.0-5.0; (2) preparing 12/204g/L ascorbic acid aqueous solution; (3) preparing dilute sulphuric acid or soluble sulfate solution, wherein the mass of sulfate ions is 0.3-1.5 times that of AgNO3; (4) at 10-60 DEG C under stirring state, mixing the dilute sulphuric acid or soluble sulfate solution and the reducing agent ascorbic acid aqueous solution with certain volume into certain volume of silver nitrate solution for reaction for 3-6 minutes, standing for 5-300 minutes and carrying out liquid-solid separation; and (5) rinsing the solid product obtained from the step (4) with deionized water and absolute ethyl alcohol respectively until the pH of the cleaning solution is neutral, and drying at 30-65 DEG C for 1.5-5 hours, thus obtaining the micro-order platy silver powder product. By adopting the preparation method, the micro-order platy silver powder which has a width-to-thickness ratio larger than or equal to 10 and plate diameter of 5-50mum; and the preparation method omits the grinding procedure of the traditional machine, is simple in technique, easy to operate, and low in cost and has no pollution to the environment.

Description

technical field [0001] The invention relates to a preparation method of micron-scale flaky silver powder, in particular to a liquid-phase reduction preparation method of micron-sized flaky silver powder with an aspect ratio ≥ 10. Background technique [0002] Silver powder is an important precious metal powder. Due to its excellent electrical and thermal conductivity, it is widely used as a raw material for electronic paste and conductive coating, and is widely used in electronic components such as electronic packaging and electrode contacts. Generally, the paste requires the particle size of silver powder to be in the micron level. [0003] Silver powder can be divided into micron-sized non-flaky silver powder and flake silver powder. [0004] There is surface contact or line contact between the flaky silver powder particles, which is much larger than the contact surface of the ultrafine non-flaky silver powder particles. Therefore, the resistance of the flaky silver powde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 田庆华郭学益焦翠燕易宇邓多
Owner CENT SOUTH UNIV
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