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Method for preparing nanometer silver powder with accurately controlled particle size

A technology of precise control and particle size, applied in the field of inorganic chemical industry, can solve the problems of inability to pre-design the product size, decrease of production efficiency, difficulty in large-scale production, etc., and achieve the effect of increasing the total silver ion concentration, simple process and stable quality

Active Publication Date: 2012-04-11
山东建邦集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some defects in the preparation of silver nanopowders by liquid phase control.
At first, most methods need to adopt control means such as organic solvent, high-temperature reaction or microwave, ultraviolet light, in aqueous solution system, normal temperature and normal pressure reaction control prepares the nano-silver powder of different sizes still is a challenge (referring to Chem.Eur.J.2005, 11, 454); Secondly, for the size control of silver powder, before the experimental results are obtained, the product size can only be qualitatively estimated (such as the size becomes larger or smaller), and the product size cannot be pre-designed and adjusted by adjusting the reaction parameters. Realize precise and quantitative controlled synthesis (referring to Acc.Chem.Res.2007,40,1067); In addition, in order to obtain nano-silver powder, control the growth of silver particles in the solution phase, often adopt the silver ion solution of low concentration, the production efficiency is obvious Drop (see CN1653907A)
Therefore, the use of liquid phase reduction technology to prepare silver nanopowder is currently difficult to achieve large-scale production in all countries in the world.

Method used

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  • Method for preparing nanometer silver powder with accurately controlled particle size
  • Method for preparing nanometer silver powder with accurately controlled particle size
  • Method for preparing nanometer silver powder with accurately controlled particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Preparation of seed crystals

[0053] Components of dispersant I: 5.0g trisodium citrate (17.0mmol)+6.7g polyvinylpyrrolidone (PVP K-30, 60.4mmol as a monomer)+18.0g sodium oleate (59.1mmol);

[0054] Reducing agent I solution: a fresh solution prepared from 225 mg sodium borohydride (5.9 mmol) and 330 mL water, wherein the concentration of sodium borohydride is about 17.9 mmol / L, and the molar ratio of sodium borohydride to silver nitrate in mixed solution I is 1:1 .

[0055] Described dispersant I and 1.0g silver nitrate (5.9mmol) are dissolved in 25.0L water and form mixed solution I (wherein the mol ratio of dispersant I and silver nitrate is 23.1: 1, the concentration of silver nitrate is about 0.2mmol / L ), under rapid stirring, then quickly add the reducing agent I solution, stir and react at room temperature for 10 minutes, and use it as a seed crystal for subsequent use.

[0056] (2) Preparation of silver-containing precursor

[0057] ① The complexing age...

Embodiment 2

[0074] (1) Preparation of seed crystals

[0075] The composition of dispersant I: 2.5g trisodium citrate (8.5mmol)+3.3g polyvinylpyrrolidone (PVP K-30, 29.7mmol in monomer)+9.0g sodium oleate (29.6mmol);

[0076] The reducing agent I solution is: a fresh solution prepared by 115mg sodium borohydride (3.0mmol) and 165mL water, wherein the concentration of sodium borohydride is about 18.4mmol / L, and the molar ratio of sodium borohydride to silver nitrate in mixed solution I is about 1:1 ;

[0077] The dispersant I and 500mg silver nitrate (2.94mmol) were dissolved in 12.5L water to form mixed solution I (wherein the mol ratio of dispersant I to silver nitrate was 23:1, and the concentration of silver nitrate was about 0.2mmol / L) , under rapid stirring, then quickly add the reducing agent I solution, stir and react at room temperature for 10 minutes, and use it as a seed crystal for later use.

[0078] (2) Preparation of silver-containing precursor

[0079] ① Prepare the mixed...

Embodiment 3

[0084] (1) Preparation of seed crystals

[0085] The composition of the dispersant I: 1.25g trisodium citrate (4.2mmol)+1.67g polyvinylpyrrolidone (PVP K-30, 15.0mmol in monomer)+4.5g sodium oleate (14.8mmol);

[0086] Reducing agent I solution: a fresh solution prepared by 56mg sodium borohydride (1.48mmol) and 82.0mL water, wherein the concentration of sodium borohydride is about 18.0mmol / L, and the molar ratio of sodium borohydride to silver nitrate in mixed solution I is about 1:1 .

[0087] Dispersant I and 250mg silver nitrate (1.47mmol) were dissolved in 6.25L water to form mixed solution I (wherein the molar ratio of dispersant I to silver nitrate was 23:1, and the concentration of silver nitrate was about 0.2mmol / L), quickly Under stirring, quickly add the reducing agent I solution, stir and react at room temperature for 10 minutes, and use it as a seed crystal for later use.

[0088] (2) Preparation of silver-containing precursor

[0089] ① Prepare the mixed solut...

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Abstract

The invention relates to a method for preparing nanometer silver powder with accurately controlled particle size, which comprises the following steps of: taking silver nitrate as a starting material, and reacting with a precipitant to form a uniform silver-containing precursor precipitate; and adding a reducing agent for reducing the silver-containing precursor precipitate while adding a silver crystal seed to obtain simple substance silver. The obtained silver powder particle is polyhedral or almost spherical, the powder body has good dispersity and uniformly distributed particle size, and particle size of the silver powder can be accurately controlled in the range of 20-300nm by controlling crystal seed size and addition. The invention is the method for preparing water solution system of nanometer silver powder which has accurately controlled particle size and is suitable for large scale production under normal temperature and normal pressure condition. The preparation method has moderate reaction condition and is simple and convenient, and the nanometer silver powder has low cost and stable quality.

Description

technical field [0001] The invention relates to a preparation method of nano-silver powder whose particle diameter can be precisely controlled, and belongs to the field of inorganic chemical industry. Background technique [0002] Metal silver has excellent physical and chemical properties, such as the best room temperature electrical conductivity, thermal conductivity, strongest reflection properties, photosensitive imaging properties, antibacterial and anti-inflammatory properties, etc., making it widely used in modern industrial fields. Silver is also the cheapest noble metal that resists high temperature oxidation. Taking advantage of its electrical and thermal conductivity, silver powder is applied to conductive paste, making it an indispensable functional material in the electronics industry. Due to the small particle size and high activity of nano-silver powder, it can effectively adjust and improve the viscosity, rheology, thixotropy and sintering activity of silver ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 陈代荣陈波焦秀玲马跃跃
Owner 山东建邦集团有限公司
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