Method capable of continuously preparing micron-sized spherical gold powder

A micron-level, gold powder technology, applied in metal processing equipment, transportation and packaging, etc., to achieve the effect of uniform particle size distribution, smooth surface and high purity

Pending Publication Date: 2022-08-02
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For gold paste users, the consistency and stability of different batches of gold paste products directly determine the quality stability of downstream products, while the batch stability of gold paste products depends on the process stability of gold powder batch preparation. Due to factors such as the development process or development cost, the research and development unit has not yet seen a publicly reported process that can be used to prepare micron-sized spherical gold powder with a narrow particle size distribution in batches. This is a technical bottleneck that must be broken through for the industrialization of domestic high-quality gold paste.

Method used

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  • Method capable of continuously preparing micron-sized spherical gold powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Using commercially available aqueous solution of chloroauric acid (impurity content ≤ 0.005wt%) as the raw material (it can also be made by adding pure gold into aqua regia and then catching the nitrification method), and using a 500mL volumetric flask to prepare gold trichloride with an Au mass concentration of 20g / L The solution is ready to use. Pour the prepared gold trichloride solution into a beaker and add about 70 mL of dilute ammonia water with a concentration of 5% dropwise with stirring at room temperature to form a gold fulminate suspension A with pH=3.5 for use.

[0039] According to the mass ratio of Au:VC:PVA=5:10:1, use 20g VC to prepare 1L of VC aqueous solution with a mass concentration of 100g / L, pour it into a 2L beaker containing 500g of PVA aqueous solution with a concentration of 2wt%, and mix and stir at room temperature. A homogeneous liquid B was formed for use.

[0040]Using the rapid rotation nucleation method, A and B were injected into a ra...

Embodiment 2

[0043] Using commercially available chloroauric acid aqueous solution (impurity content ≤ 0.005wt%) as raw material (it can also be made by adding pure gold into aqua regia and then catching nitrification method), using a 1L volumetric flask to configure gold trichloride with Au mass concentration of 25g / L The solution is ready to use. The prepared gold trichloride solution was poured into a beaker, and about 130 mL of ammonia water with a concentration of 8% was added dropwise with stirring at room temperature to form a gold fulminate suspension A with pH=3.7 for use.

[0044] According to the mass ratio of Au:VC:PVA=5:10:1.1, prepare 2L of VC aqueous solution with a mass concentration of 100g / L with 200g VC, pour it into a 5L beaker containing 440g of PVA aqueous solution with a concentration of 5wt%, and mix and stir at room temperature , to form a homogeneous liquid B for use.

[0045] Using the rapid rotation nucleation method, A and B were simultaneously injected into a...

Embodiment 3

[0048] Using commercially available aqueous solution of chloroauric acid (impurity content ≤ 0.005wt%) as raw material (it can also be made by adding pure gold into aqua regia and then catching the nitrate method), using a 1L volumetric flask to configure gold trichloride with Au mass concentration of 30g / L The solution is ready to use. The prepared gold trichloride solution was poured into a beaker, and about 200 mL of ammonia water with a concentration of 6% was added dropwise with stirring at room temperature to form a gold fulminate suspension A with pH=4.0 for use.

[0049] According to the mass ratio of Au:VC:PVA=5:10:1.2, use 300g VC to prepare 3L of VC aqueous solution with a mass concentration of 100g / L, pour it into a 5L beaker containing 720g of PVA aqueous solution with a concentration of 5wt%, and mix and stir at room temperature , to form a homogeneous liquid B for use.

[0050] Using the rapid rotation nucleation method, A and B were sprayed into a fast rotatin...

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Abstract

The invention provides a method capable of continuously preparing micron-sized spherical gold powder with uniform particle size. According to the method, a rapid rotation nucleation method capable of effectively reducing interference of the external environment on gold grain nucleation is adopted, the gold-containing mother liquor and a reducing agent are introduced into a rapid rotation nucleation reactor at the same time, mass transfer reaction is rapidly completed in micro-nano liquid drops generated through high-speed rotation cutting, a huge amount of uniform crystal nuclei are formed, then the crystal nuclei are introduced into a rear reactor, and the gold-containing mother liquor is obtained. And the controllable growth of the spherical gold powder crystal grains is continuously completed until the spherical gold powder particles in the micron-sized particle size range are obtained, then the obtained micron-sized spherical gold powder precipitate is washed and dried, and the spherical gold powder with the uniform particle size can be obtained. The spherical gold powder which is high in purity, good in dispersity, smooth in surface and more uniform in particle size distribution compared with a common liquid phase reduction method can be continuously prepared through the method, and the average particle size D50 of the spherical gold powder ranges from 1 micrometer to 3 micrometers.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a method for continuously preparing micron-sized spherical gold powder for electronic paste. Background technique [0002] With the rapid development of advanced manufacturing industries such as 5G communications, radar electronics, and smart cars in the electronic information industry, the market is increasingly interested in electronic components such as hybrid multi-chip modules (MCM-C / D), microwave hybrid integrated circuits, and high-power micro-assembled chips. Demand has also exploded. Since gold has electrical conductivity second only to silver and copper, excellent corrosion resistance and oxidation resistance, and gold usually has no electromigration, these points jointly determine the preparation of high-frequency, high-frequency, high-frequency, Due to the inherent advantages of low-loss and long-life electronic components, gold conductor paste has becom...

Claims

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Application Information

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IPC IPC(8): B22F1/05B22F1/065B22F9/24
CPCB22F9/24
Inventor 罗君王琰诏郝红蕊杨志民陈峤赵彦弘杨剑
Owner GRIMAT ENG INST CO LTD
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