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A kind of preparation method of nanometer or submicron silver particle powder

A technology of submicron and silver particles, which is applied in the field of nanoscale sheet-like agglomerated silver particle powder or submicron spherical silver particle powder, based on the liquid phase reduction method of sodium hypophosphite system to prepare nanoscale spherical silver particle powder, It can solve the problems of complex reaction solution, cumbersome post-treatment process, and the unit output needs to be improved, and achieve the effect of high purity, good shape and size uniformity, and easy washing

Active Publication Date: 2016-06-01
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent whose publication number is CN101254541A discloses a preparation and storage method of nano-silver powder for conductive adhesive. Stock solution, the pH value of the reaction system is adjusted by sulfuric acid, the silver nitrate solution is added dropwise to the reducing agent solution under the condition of reaction temperature of 40-45°C and magnetic stirring, and silver powder with a particle size of 30-50 nanometers is prepared. The reaction solution of the method is relatively complicated, the post-treatment process is cumbersome, and the unit output of silver powder still needs to be improved

Method used

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  • A kind of preparation method of nanometer or submicron silver particle powder
  • A kind of preparation method of nanometer or submicron silver particle powder
  • A kind of preparation method of nanometer or submicron silver particle powder

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Weigh 0.5g of silver nitrate and dissolve it in 10ml of deionized water to make a silver nitrate solution, add 0.1ml of nitric acid into the silver nitrate solution under stirring, and then add 5ml of ethanol to obtain the mixed solution as the oxidation solution; weigh 0.4g Sodium hypophosphite (NaH 2 PO 2 ) into 2.5ml of deionized water, and after complete dissolution, add 2.5ml of ethanol to the sodium hypophosphite solution as a reducing solution. Quickly add the reducing solution to the oxidizing solution at 20°C and 300 rpm under stirring conditions, stop stirring after mixing evenly, let stand for reaction for 40 minutes, centrifuge after the reaction is completed, collect the precipitate, and wash it with deionized water for four weeks. The second time is washed twice with ethanol, and finally dried in vacuum at low temperature to obtain nano-scale spherical silver particle powder.

[0038] Such as figure 1 As shown in the scanning electron micrograph, the pa...

Embodiment 2

[0040] It is basically the same as Example 1, except that distilled water is used instead of deionized water, and acetone is used instead of ethanol. Observation by scanning electron microscope shows that the particle size of the obtained nano-scale spherical silver particle powder is concentrated between 30 and 100 nanometers.

Embodiment 3

[0042] Weigh 0.5g of silver nitrate and dissolve it in 5ml of deionized water to prepare a silver nitrate solution, add 0.015ml of nitric acid into the silver nitrate solution under stirring, and the resulting mixed solution is used as an oxidation solution; weigh 0.25g of sodium hypophosphite (NaH 2 PO 2 ) into 10ml of deionized water, and after it is completely dissolved, add 5ml of ethanol to the sodium hypophosphite solution as a reducing solution. Quickly add the oxidizing solution to the reducing solution at 20°C and 300 rpm under stirring conditions, stop stirring after mixing evenly, let stand for reaction for 40 minutes, centrifuge after the reaction is completed, collect the precipitate, and wash it with deionized water for four weeks. The second time is washed twice with ethanol, and finally dried in vacuum at low temperature to obtain nano-scale spherical silver particle powder. Observation by a scanning electron microscope shows that the particle size of the obta...

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Abstract

The invention relates to a preparation method of nano or sub-micron silver particle powder. The preparation method is based on the sodium hypophosphite liquid phase reduction method to prepare the nano or sub-micron silver particle powder. The preparation method is characterized in that water is used as solvent, inorganic acid, organic acid or salts are used as a main shape and size modifying agent, organic solvent is used as a dispersive agent or an auxiliary shape and size modifying agent, and sodium hypophosphite is used as a reduction agent. The preparation method has the advantages that any surface active agent is not used, so the washing of products is easy, and the purity is high; nano similar-spherical silver particle powder, nano flaky agglomeration silver particle powder or sub-micron similar-spherical silver particle powder can be obtained; the shape and size uniformity of the silver particle powder prepared by the method is good, the purity of the silver powder is high, the yield rate and unit output of silver are high, and the preparation method can be applied to the fields of conductive slurry, conductive glue, electric contact material, catalyzing and the like.

Description

technical field [0001] The present invention relates to a preparation method of nanometer or submicron silver particle powder, in particular to a preparation method based on sodium hypophosphite system liquid phase reduction method to prepare nanoscale spherical silver particle powder, nanoscale flake-like agglomerated silver particle powder or submicron A method for class-like spherical silver particle powder. Background technique [0002] Nano or submicron metal silver particle powder can be widely used in conductive paste, conductive adhesive, electrical contact materials, catalysis, antibacterial, electromagnetic protection and other fields. [0003] At present, the methods for preparing nanometer or submicron silver particle powder mainly include thermal decomposition method, electrochemical method and chemical reduction method at home and abroad. The shape of the prepared nanometer or submicron silver particle powder is generally spherical or quasi-spherical, and ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
Inventor 刘春艳聂士东张志颖
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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