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A kind of preparation method of high tap density silver powder

A technology of tap density and silver powder, which is applied in the field of preparation of high tap density silver powder, can solve the problems of expensive chloroplatinic acid reagent, limited application, complicated process flow, etc., and achieves the effects of low price, reduced production cost, and simplified process flow

Active Publication Date: 2015-10-07
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent document CN1401452A discloses "preparation of hexagonal flaky silver powder by chemical reduction method", which uses hydrogen peroxide as a reducing agent, which is more environmentally friendly; but this process needs to add PVP as a dispersant, and also needs to add chloroplatinic acid to catalyze, and the reduction system is Polyol-ammonia silver compound; the use of multiple reagents makes the process complicated, and the chloroplatinic acid reagent is expensive, which limits its application in this process

Method used

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  • A kind of preparation method of high tap density silver powder
  • A kind of preparation method of high tap density silver powder
  • A kind of preparation method of high tap density silver powder

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Prepare 1000mL of 50g / L silver nitrate solution, add concentrated ammonia water with a mass percentage concentration of 25-28% to it to obtain a silver ammonia solution with a pH=11.0; then measure 100mL of a 30% mass percentage concentration of hydrogen peroxide solution, And add water to it to dilute the hydrogen peroxide to 1000mL;

[0031] Use 200ml of deionized water as the bottom solution, heat the deionized water bath to 30°C; within 20s, add the silver ammonia solution and hydrogen peroxide solution into the bottom solution in parallel while fully stirring, react for 30min, and pass the concentration of 1mol / L NaOH solution to maintain the pH value in the reaction system throughout the process at 8.0-9.5. Then filter the reacted solution to obtain silver powder, wash the obtained silver powder 3 times with deionized water, and then wash 3 times with absolute ethanol; finally put the silver powder in a vacuum drying oven at 40°C and -0.08MPa Let dry for 10 hour...

Embodiment 2

[0034] Prepare 1000mL of 40g / L silver nitrate solution, add concentrated ammonia water with a mass percentage concentration of 25-28% to it to obtain a silver ammonia solution with a pH=10.5; measure 120mL of a 30% mass percentage concentration of hydrogen peroxide solution, and add Add water to dilute the hydrogen peroxide to 700mL;

[0035] Use 100mL deionized water as the bottom solution, heat the deionized water bath to 20°C, within 15s, add the silver ammonia solution and hydrogen peroxide solution into the bottom solution in parallel flow while fully stirring, react for 20min, and pass the concentration The 1.5 mol / L NaOH solution keeps the pH value of the reaction system in the whole process in the range of 8.0-9.5. Then the solution after the reaction is filtered to obtain silver powder, the silver powder obtained is cleaned 4 times with deionized water, and then cleaned 3 times with absolute ethanol, and finally the obtained silver powder is dried in a vacuum oven at ...

Embodiment 3

[0038] Prepare 1000mL of 30g / L silver nitrate solution, add concentrated ammonia water with a mass percentage concentration of 25-28% to it to obtain a silver ammonia solution with a pH=11.5; measure 40mL of a 30% mass percentage concentration of hydrogen peroxide solution, and Add water to it to dilute the hydrogen peroxide to 400mL;

[0039] Take 100mL deionized water as the bottom solution, heat the deionized water bath to 50°C, and within 30s, add the silver ammonia solution and hydrogen peroxide solution into the bottom solution while fully stirring, and react for 15 minutes, and by adding the concentration of 2mol / L NaOH keeps the pH value of the reaction system in the whole process in the range of 8.0-9.5. Then the solution after the reaction is filtered to obtain silver powder, the silver powder obtained is cleaned 3 times with deionized water, and then cleaned 2 times with absolute ethanol, and finally the cleaned silver powder is dried in a vacuum drying oven at 75°C...

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Abstract

The invention relates to a preparation method of a high-tap-density silver powder. The preparation method specifically comprises the following steps that (1) an ammoniacal silver nitrate solution at a certain PH value is prepared, (2) a hydrogen peroxide solution in certain concentration is prepared, (3) deionized water serves as a base solution, the ammoniacal silver nitrate solution and the hydrogen peroxide solution are added into the base solution and react within the range of certain PH values, (4) a product is settled, filtered, washed and dried. Compared with the prior art, the preparation method has the advantages that dispersing agents or protective agents do not need to be added in the reaction process, the zeta potential on the surface of the silver powder is adjusted simply by adjusting the pH of a solution system, and agglomeration of the silver powder is prevented. The silver powder prepared through the method is good in dispersity and high in crystallinity degree and tap density; in addition, the technology procedure is simple, operation is simple and convenient, reducing agents are environmentally friendly, and the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to a preparation method of high tap density silver powder. Background technique [0002] Silver powder is the most widely used precious metal powder in the electronics industry, and it is used to make various electronic pastes, conductive adhesives, etc. When silver powder is used to prepare electronic paste, in order to ensure the good conductivity of the thick film integrated circuit prepared by it, the silver powder is required to have good high temperature shrinkage resistance, that is, the silver powder is required to have high crystallinity and high tap density. [0003] At present, there are many methods for preparing silver powder; among them, the liquid phase reduction method is widely used because of its simple equipment, mild process conditions and low cost. In order to prevent the agglomeration of silver powder, dispersants or protective agents are added to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/00B22F9/24
Inventor 郭学益田庆华邓多焦翠燕易宇
Owner CENT SOUTH UNIV
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