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Preparation method for inductively producing silver powder by using micro-nano bubbles as crystal seeds

A technology of micro-nano bubbles and silver powder is applied in the field of materials, which can solve the problems of high cost and low yield, and achieve the effects of good crystal nucleus growth rate and good reduction rate.

Active Publication Date: 2016-08-10
SUZHOU SMART ADVANCED COATING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the problem of high cost and low yield in the physical method, the widely used chemical liquid phase reduction method is to reduce the salt solution or oxide containing silver ions to silver by chemical reaction. For example, the patent CN2014 10394624. Metal salt, the method that adopts liquid phase reduction method to generate silver powder

Method used

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  • Preparation method for inductively producing silver powder by using micro-nano bubbles as crystal seeds
  • Preparation method for inductively producing silver powder by using micro-nano bubbles as crystal seeds
  • Preparation method for inductively producing silver powder by using micro-nano bubbles as crystal seeds

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Effect test

Embodiment 1

[0031] Embodiment 1 (silver powder S001)

[0032] (1) Preparation of oxidant solution containing silver nitrate solution, silver nitrate solid or equivalent silver nitrate liquid is dissolved in deionized water, and the molar concentration of silver ions in the solution [silver ion]=0.3mol / l is kept, and the solution is kept for 20-20 mol / l. 30°C constant temperature state;

[0033] (2) The reducing agent solution containing hydrazine hydrate is prepared, and the hydrazine hydrate solution is added in deionized water to make, according to the silver content in the silver-containing oxidant solution, keep the molar ratio [silver ion]:[hydrazine hydrate]=1 in the solution: 0.1~5, keep the solution at a constant temperature of 10~50°C;

[0034] (3) Preparation of dispersant solution: add one or more than two kinds of PVP or polyethylene glycol 400 to dissolve in deionized water, the content of which is 50-100g / l, stir well, and keep the solution at a constant temperature of 10-5...

Embodiment 2

[0036] Embodiment 2 (silver powder S002)

[0037] Preparation of oxidant solution: prepare 500ml of silver nitrate solution containing 180g / L of silver in a 2000ml wide-mouth bottle, add 200ml of ammonia water with a mass percentage concentration of 18% to it to obtain silver ammonia solution, and heat it to 45°C for later use;

[0038]Preparation of reducing agent solution: prepare a solution containing vitamin C and hydroxylamine sulfate in another 2000ml jar: dissolve 50g of hydroxylamine sulfate and 50g of vitamin C in 500ml of deionized water, heat to 45°C for later use;

[0039] Dispersant solution preparation: Dispersant solution prepared in a 500ml jar: dissolve 65g of PVP and 40ml of Tween 40 in 250ml of deionized water, heat to 35°C for later use;

[0040] Use a metering pump to pre-pour the dispersant solution into a 5000ml wide-mouth bottle, and at the same time turn on the micro-nano bubble generator to generate controllable micro-nano bubbles in the dispersant so...

Embodiment 3

[0041] Embodiment 3: batch production (silver powder S003)

[0042] Add 250 kg of silver nitrate solid in a 1000L preparation tank, add 800L of deionization, fully stir and dissolve, then add 250L of ammonia water with a mass percentage concentration of 23% to obtain a silver ammonia solution, heat to 35°C for later use (oxidant solution) ;

[0043] Add 500L of deionized water into another 1000L preparation tank, then add 150 kg of vitamin C and 55 kg of hydroxylamine sulfate, fully dissolve and heat to 35°C for standby (reducing agent solution);

[0044] Dissolve 35kg of PVP in 400L of deionized water in a 500L preparation tank, stir well, and heat to 35°C for later use (dispersant solution);

[0045] Use a metering pump to inject the dispersant solution into the 3000L reaction kettle in advance, and at the same time turn on the micro-nano bubble generator to generate controllable micro-nano bubbles in the dispersant solution in the reaction kettle, and then quantitatively p...

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Abstract

The invention discloses a preparation method for inductively producing spherical and sphere-like silver powder by using micro-nano sized bubbles as crystal seeds. The preparation method specifically includes the steps that a prepared dispersing agent solution is added into a reaction kettle in advance, a micro-nano bubble generator is started, and the controllable micro-nano bubbles (0.1-900 nm) are generated in the dispersing agent solution in the reaction kettle; then, a prepared oxidation solution (an aqueous solution containing silver ions or a silver-ammonia solution) and a prepared reduction solution (an aqueous solution containing one or more of hydroxylamine compounds or vitamin C or formaldehyde or hydrazine hydrate) are added at the same time, and a reduction reaction is performed under violent stirring; and the micro-nano bubbles pre-generated in the dispersing agent solution are used as the crystal seeds, and the micro-nano bubble crystal seeds can effectively control the particle size of reduced silver particles in the whole reduction reaction process. According to the method disclosed by the invention, the particle size of the particles in the production process of the silver powder can be controlled effectively, and meanwhile the crystal nucleus growing speed and dispersity are well controlled; the produced silver powder has quite good crystallinity and sphericity, high vibratory compaction performance and high dispersity; and particularly, loose structures in the particles of the silver powder are of great help to the activity of the silver powder.

Description

technical field [0001] The invention relates to the field of material technology, in particular to a preparation method of micron-sized silver powder. Background technique [0002] Silver powder is widely used in solar energy, electronic components manufacturing, electroplating, battery and chemical catalysis, jewelry and other industries. With the development of electronic components in the direction of miniaturization and high performance, higher requirements are put forward for performance indicators such as sintering activity, dispersibility, sphericity, and crystallinity of silver powder. At present, the preparation methods of silver powder include physical methods and chemical methods, and physical methods include atomization method, vapor phase evaporation condensation method, grinding method and the like. Chemical methods mainly include liquid phase reduction method, electrochemical deposition method, electrolysis method and so on. Due to the problem of high cost a...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/05
CPCB22F9/24B22F2009/245B22F1/05B22F1/056B22F2998/10C22C5/06B22F1/07
Inventor 龚强
Owner SUZHOU SMART ADVANCED COATING TECH CO LTD
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