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Sphere-like silver powder with particle size capable of being accurately controlled and preparation method thereof

A technology with precise control and spherical shape, which is applied in metal processing equipment, transportation and packaging, etc., can solve the problems that are not suitable for large-scale industrial production, the particle size cannot be precisely controlled, and the adjustable range of particle size is narrow, so as to achieve easy scale-up and industrialization. Chemical application, wide controllable range of particle size and uniform shape

Inactive Publication Date: 2021-03-12
山东建邦胶体材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a long period, low crystallinity of silver powder, uneven appearance, narrow adjustable range of particle size, inability to precisely control particle size, complicated operation, and the need to complete the reaction in a certain pressure vessel and high temperature, which is not suitable for large-scale industrial production. There is a certain operational risk

Method used

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  • Sphere-like silver powder with particle size capable of being accurately controlled and preparation method thereof
  • Sphere-like silver powder with particle size capable of being accurately controlled and preparation method thereof
  • Sphere-like silver powder with particle size capable of being accurately controlled and preparation method thereof

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preparation example Construction

[0041] The present application uses nano-silver colloid as a seed crystal. The particle size of silver particles in the nano-silver colloid is 50-300nm, the content of silver particles is 0.5-4%, and the silver particles have a hydrophilic surface. As long as the nano-silver colloids meeting the above conditions can be used as the seed crystals of this application. Specifically, the nano-silver glue used in the following examples refers to the patent CN102407342B, and the preparation method of the nano-silver glue specifically includes the following steps:

[0042] (1) Preparation of seed crystals

[0043]The polymer is calculated as a monomer. Dissolve the dispersant I and silver nitrate in water at a molar ratio of 1 to 100:1 to form a mixed solution I with a silver nitrate concentration of 0.01 to 20.0 mmol / L, and then add the reducing agent I under stirring. solution, continue to stir and react to form nano-silver seeds;

[0044] Wherein, the dispersant I is one or a com...

Embodiment 1

[0057] Embodiment 1 preparation target particle diameter D50 is the spherical silver powder 1# of 0.5 μ m

[0058] The specific preparation method of described quasi-spherical silver powder comprises the following steps:

[0059] (1) Take by weighing 4.5Kg silver nitrate solid, be mixed with the silver nitrate solution A of 1mol / L and add nitric acid, adjust to pH to 2; Take 5Kg ascorbic acid as reducing agent, be mixed with reducing agent solution B of 1.5mol / L And add ammonia water to adjust the pH to 5; weigh 3.2Kg polyvinylpyrrolidone, and prepare a dispersant solution C with a concentration of 250g / L.

[0060] (2) take by weighing 300g particle diameter and be the above-mentioned seed crystal of 50nm (wherein silver particle content is 1.0%, and silver particle has hydrophilic surface), after adding in the dispersant solution C and stirring, keep the reaction kettle temperature to be 15 ℃, The stirring speed is 200r / min, and the silver nitrate solution A and the reducing...

Embodiment 2

[0065] Embodiment 2 Preparation target particle diameter D50 is the spherical silver powder 2# of 0.8 μ m

[0066] The specific preparation method of described quasi-spherical silver powder comprises the following steps:

[0067] (1) Take by weighing 4.5Kg silver nitrate solid, be mixed with the silver nitrate solution A of 1mol / L and add nitric acid, adjust to pH to 2; Take 5Kg glucose and make reducing agent, be mixed with reducing agent solution B of 2mol / L and Add sodium hydroxide to adjust the pH to 5; weigh 3.2Kg of polyvinylpyrrolidone, and prepare a dispersant solution C with a concentration of 250g / L.

[0068] (2) take by weighing 300g particle diameter and be the above-mentioned seed crystal of 100nm (wherein silver particle content is 1.5%, and silver particle has hydrophilic surface), after adding in the dispersant solution C and stirring, keep the reaction kettle temperature to be 20 ℃, The stirring speed is 200r / min, and the silver nitrate solution A and the red...

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Abstract

The invention provides sphere-like silver powder with particle size capable of being accurately controlled and a preparation method thereof. The method comprises the following steps: (1), mixing a nano-silver colloid with a dispersing agent solution to obtain a mixed solution, wherein the silver particles in the nano-silver colloid are approximately spherical; (2) under a stirring condition, dripping a silver salt solution and a reducing agent solution into the mixed solution in the step (1) in a parallel flow mode to react, so as to obtain silver powder slurry; and (3) carrying out solid-liquid separation, washing and drying on the silver powder slurry obtained in the step (2) to obtain the sphere-like silver powder. The silver salt solution and the reducing agent solution are dropwise added into the mixed solution of a dispersing agent and a seed crystal in a parallel flow mode to control the generation speed of elemental silver, so that the elemental silver uniformly grows on the provided nano-silver colloid seed crystal, the sphere-like silver powder with the particle size accurately controllable is obtained, and the reaction conditions are mild, normal temperature and normal pressure are achieved, equipment and process are simple, and the production period is short; it is easy to amplification and industrial application; the prepared silver powder is uniform in morphology,good in dispersity and high in tap density.

Description

technical field [0001] The invention relates to a preparation method of silver powder, in particular to a spherical silver powder whose particle size can be precisely controlled and a preparation method thereof. Background technique [0002] Silver powder has excellent electrical and thermal conductivity, and is widely used in the fields of solar cell paste, conductive adhesive and other electronic pastes. With the depletion of non-renewable resources such as oil and coal, and the enhancement of people's awareness of environmental protection, the development of new energy has attracted more and more attention, especially the development and utilization of solar energy has become a hot spot. Silver powder is the conductive phase of the silver paste of crystalline silicon solar cells, accounting for about 90% by mass in the silver paste, which has a great influence on the rheological properties and printability of the paste, and at the same time plays a decisive role in the ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00
CPCB22F9/24B22F1/065
Inventor 陈波许文艳马跃跃王艳云陈朋韩世生
Owner 山东建邦胶体材料有限公司
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