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Preparation method of low-burnout rate flake silver powder

A flake silver powder and silver powder technology, which is applied in the field of flake silver powder preparation by mechanical ball milling, can solve the problems of low flake degree, high burning loss rate, and surface adsorption of flake silver powder, and achieve high flake degree and low fever small effect on loss rate, electrical conductivity and physical properties

Inactive Publication Date: 2013-04-10
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problems of high burning loss rate and low degree of flaking, the object of the present invention is to provide a method for preparing flaky silver powder with low burning loss rate, aiming to solve the related problems of surface adsorption of flaky silver powder prepared by mechanical ball milling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A. 10.00g of spherical silver powder with a purity of 99.99% is used as raw material, mixed with 0.50g of oleic acid and 0.10g of calcium stearate (according to the mass ratio of spherical silver powder: ball milling aid: dispersant = 100: 5: 1), add Adjust the solution with ionized water until the concentration of the ball milling aid is 20g / L, and the concentration of the dispersant is 4g / L to obtain a mixed solution;

[0019] B. Ball mill the mixed solution obtained in step A for 15 hours at a rotational speed of 200 r / min, wash with deionized water and absolute ethanol three times each, then filter with suction and dry at 80°C for 6 hours to obtain a low-burning rate tablet silver powder.

[0020] The obtained flaky silver powder with low burning loss rate has good dispersibility, average particle size of 12.83 μm, bulk density of 0.823 g / ml, and burning loss rate of 0.50%.

Embodiment 2

[0022] A. Take 99.99% spherical silver powder 10.00g as raw material, mix with 0.30g stearic acid and 0.10g lecithin (according to the mass ratio of spherical silver powder: ball milling aid: dispersant = 330: 3: 1), add deionized Adjust the solution with water until the milling aid concentration is 30g / L, and the dispersant concentration is 10g / L to obtain a mixed solution;

[0023] B. The mixed solution obtained in step A was ball-milled for 20 h at a rotational speed of 250 r / min, washed once with absolute ethanol and twice with deionized water, then suction-filtered, and dried at 60°C for 8 h, namely Obtain flake silver powder with low burning loss rate.

[0024] The obtained flaky silver powder with low burning loss rate has good dispersibility, average particle size of 10.58 μm, bulk density of 1.045 g / ml, and burning loss rate of 0.48%.

Embodiment 3

[0026] A. Take 10.00 g of spherical silver powder with a purity of 99.99% as a raw material, mix it with 0.80 g of absolute ethanol and 0.10 g of castor oil (according to the mass ratio of spherical silver powder: ball milling aid: dispersant = 100: 8: 1), add Adjust the solution with ionized water until the concentration of ball milling aid is 40g / L, and the concentration of dispersant is 5.0g / L;

[0027] B. The mixed solution obtained in step A was ball-milled for 15 h at a rotational speed of 300 r / min, washed once with deionized water and twice with absolute ethanol, then suction-filtered, and dried at a temperature of 60 °C for 8 h, namely Obtain flake silver powder with low burning loss rate.

[0028] The obtained flaky silver powder with low burning loss rate has good dispersibility, average particle size of 8.13 μm, bulk density of 0.891 g / ml, and burning loss rate of 0.32%.

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Abstract

The invention provides a preparation method of low-burnout rate flake silver powder. In the method, spherical silver powder is utilized as a raw material. The method comprises the following steps: mixing the spherical silver powder, ball milling assistant and dispersant according to a weight ratio of 50-400:1-20:0.05-10, and adding de-ionized water to regulate the solution until the concentrationof the ball milling assistant is 10-200 g / L and the concentration of the dispersant is 0.5-100 g / L; carrying out ball milling on the mixed solution at a rotation speed of 100-400 r / min for 5-80 h, respectively washing with anhydrous alcohol and de-ionized water for 1-3 times, then filtering in vacuum, and drying at 30-120 DEG C for 4-20 h to obtain the low-burnout rate flake silver powder. The prepared powder has the advantages of large radius-thickness ratio, low loose density, good conductibility, low burnout rate, high flaking degree and good dispersibility, the particle size of the powderis 3.91-17.05 mu m, the specific area is 0.404-1.762 m<2> / g, the loose density is 0.871 m<3> / g, the tap density is 1.127 m<3> / g, and the burnout rate is 0.01-0.20%. Thus, the flake silver powder is well applicable to electronic paste appliances in the later period.

Description

technical field [0001] The invention relates to a method for preparing flaky silver powder by a mechanical ball milling method, in particular to a method for preparing flaky silver powder with low burning loss rate and low bulk density. Background technique [0002] As precious metal pastes are widely used in the microelectronics industry, various properties of precious metal powders are subject to special requirements. As an important conductive functional material for conductive paste, the demand for ultrafine silver powder is increasing continuously, and there are requirements for the performance of silver powder such as purity, particle size, dispersibility, morphology, specific surface area, square resistance, burning loss rate and other indicators. Flake silver powder is widely used in single-sided capacitors, filters, carbon film potentiometers, tantalum capacitors, membrane switches, semiconductor chips and other electronic components. In order to adapt to the devel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/04
Inventor 严继康甘国友张磊郑娅朱华杜景红易健宏
Owner KUNMING UNIV OF SCI & TECH
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