Surface modified particle diameter mixed silver powder and preparation method thereof

A technology of surface modification and surface modifier, applied in the field of silver powder for solar cell electrode paste, can solve the problems of uncertain proportion, difficult industrialization, unstable molecular weight, and unstable performance.

Active Publication Date: 2012-04-11
ZHEJIANG GUANGDA ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although surface-modified silver powder can be obtained, it has the following disadvantages: the surface of silver powder is coated with a variety of organic substances, the proportion is uncertain, and the influence on the performance of the slurry is not stable; it belongs to the liquid phase-mechanical method, the process is complicated, and the production cycle is long; ball milling Will produce uncertain deformation, general controllability
[0005] Chinese patent CN15857833A discloses a preparation method of silver powder in printing paste for solar cell electrodes, discloses a preparation method of silver powder with a particle size of 0.2-1 μm, and the reduction reaction process is carried out in N 2 In the atmosphere, mass production is difficult and the cost is high; gelatin is added as a protective agent in the reaction process. In fact, gelatin is soluble in water, but insoluble in most organic solvents, and has poor compatibility with organic carriers. Gelatin is a natural extract. The molecular weight and performance are unstable, and the silver powder obtained by reducing the water-based polymer as a protective agent is easy to suspend in the aqueous solution, and the solid-liquid separation is quite difficult, which is difficult for industrialization

Method used

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  • Surface modified particle diameter mixed silver powder and preparation method thereof
  • Surface modified particle diameter mixed silver powder and preparation method thereof
  • Surface modified particle diameter mixed silver powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 157gAgNO 3 Dissolve in 1L of water, stir to dissolve to obtain silver solution (1); add 1g terpineol to 200ml ethanol, stir and mix evenly to obtain solution (2); 20% sodium hydroxide solution as solution (3); Add 60g of hydrazine hydrate (50%) to 1L of water, add nitric acid to adjust the pH to 8, and obtain a reducing solution. Control the reaction temperature at 35±2°C, add (1) (2) (3) to (4) within 30 minutes at the same time, turbine-type stirring paddle, stirring speed 500RPM, stir for 10 minutes after the addition is completed, and finally control the pH value 14, then let it stand for precipitation, collect the precipitated powder, wash the powder with deionized water until the conductivity of the filtrate is not greater than 20μs / cm, filter and dry at 60°C, grind and sieve to obtain surface modified particle size mixed silver powder, powder The detection performance is shown in Table 1.

Embodiment 2

[0033] 157gAgNO 3 Dissolve in 1L of water, stir to dissolve to obtain silver solution (1); add 0.5g n-hexanol to 100ml ethanol, stir and mix well to obtain solution (2); 20% ammonia solution as solution (3); hydrate 60g Hydrazine (50%) was added to 1L of water, and sodium hydroxide was added to adjust the pH value to 12 to obtain a reducing solution. Control the reaction temperature at 40±2°C, add (1)(2)(3) to (4) within 50min at the same time, the turbine type stirring paddle, the stirring speed is 200RPM, and then stir for 10min after the dropwise addition is completed, and the final pH value is controlled 8.5, then let it stand for precipitation, collect the precipitated powder, wash the powder with deionized water until the conductivity of the filtrate is not greater than 20 μs / cm, filter and dry at 60°C, grind and sieve to obtain surface modified particle size mixed silver powder, powder The body detection performance is shown in Table 1.

Embodiment 3

[0035] 157gAgNO 3 Dissolve in 1L of water, stir to dissolve to obtain silver solution (1); add 4g of butyl acetate to 100ml of ethanol, stir and mix evenly to obtain solution (2); 30% aqueous nitric acid solution as solution (3); add 90g of ascorbic acid Add it to 1L of water, stir to dissolve and adjust the pH to 8 with sodium hydroxide to obtain a reducing solution. Control the reaction temperature at 40±2°C, add (1)(2)(3) to (4) within 100min at the same time, the turbine type stirring paddle, the stirring speed is 500RPM, and then stir for 10min after the dropwise addition is completed, the final pH value The control is 3, solid-liquid separation, collecting the precipitated powder, washing the powder with deionized water until the conductivity of the filtrate is not greater than 20μs / cm, drying at 50°C after filtering, pulverizing and sieving to obtain a surface-modified particle size mixed silver powder, powder The body detection performance is shown in Table 1.

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Abstract

The invention provides surface modified particle diameter mixed silver powder and a preparation method thereof. The preparation method comprises the following steps of: adding an alcoholic solution containing 0.3-3.0mol / L of silver nitrate aqueous solution, a pH modifier and an alcohol or ester surface modifier into a reducing solution containing hydrazine monohydrate or ascorbic acid in a parallel flow mode; under a high-shear stirring action, reacting for 20-100min in a stainless steel reaction kettle; regulating reaction temperature to be 20-50DEG C and the pH value to be 1-14 to select a control range; reducing precipitated silver powder in one step; synchronously carrying out surface treatment on silver powder surface, wherein the silver powder is quickly precipitated because the surface of the silver powder is non-hydrophilic, and solid and liquid are extremely easy to separate; washing with deionized water; drying at 50-80DEG C; and smashing and screening to obtain the surface modified silver powder. The preparation method of the silver powder is characterized in that the particle diameter can be adjustably changed between the nanometer / micron scale and the micron / micron scale. The silver powder obtained with the preparation method has the advantages of good silver powder dispersibility, high tap density, good filling property and good affinity solubility with an organic carrier, is extremely easy to disperse in slurry to form silver paste with high solid content, and is especially suitable for pouring in holes and for solar cell silver paste.

Description

technical field [0001] The invention belongs to the field of metal powder processing, and specifically provides a method for preparing a surface-modified particle-size mixed silver powder and a surface-modified particle-size mixed silver powder, which is used for silver powder for electronic paste, and particularly relates to a solar cell electrode paste Use silver dust. Background technique [0002] As the most commonly used conductive material for electronic paste, ultra-fine silver powder is not only used in traditional component electrode paste and hybrid integrated circuit paste, but also in new application fields including solar cell paste, RFID silver paste, PDP silver paste, etc. Therefore, its preparation technology has been greatly developed. Liquid phase method, solid phase method and gas phase method are all used for research, but the most commonly used and most economical large-scale production method is still the liquid phase reduction method. The traditional ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00
Inventor 孟淑媛黄月剑
Owner ZHEJIANG GUANGDA ELECTRONICS TECH
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