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Micron-sized spherical hollow gold powder and preparation method therefor

A micron-scale, spherical technology that can be used in metal processing equipment, transportation and packaging to solve problems such as large shrinkage, foaming, and reduced slurry viscosity stability.

Active Publication Date: 2020-10-23
西安宏星电子浆料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, due to the large shrinkage of high-temperature sintering, the flake gold powder is generally not used in thick-film gold paste and low-temperature co-fired ceramics (LTCC) inner and outer layer gold paste products, and commercially available spherical gold powder has a relatively large tap density (generally 7 -8.5g / cm3), there is a phenomenon that the gold paste is separated after being placed for a period of time, resulting in poor film density after the gold paste is sintered and affecting the reliability of military electronic components
Patent document CN101433959A discloses a preparation method of hollow nano-gold powder material, which uses cobalt as a sacrificial template to prepare hollow nano-gold powder. Due to the presence of cobalt, the nano-gold powder is easily polluted and affects its use in gold paste. , and the nano-scale gold powder is easy to reduce the viscosity stability of the slurry due to its small particles, and the foaming is serious after sintering

Method used

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  • Micron-sized spherical hollow gold powder and preparation method therefor
  • Micron-sized spherical hollow gold powder and preparation method therefor
  • Micron-sized spherical hollow gold powder and preparation method therefor

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preparation example Construction

[0047] The preparation method of micron spherical hollow gold powder of the present invention comprises the following steps:

[0048] (1) Adjust the pH value of the chloroauric acid solution to 4~5;

[0049] (2) Add the alcohol solution of the dispersant to the solution obtained in step (1), and stir evenly, wherein the dispersant is selected from C6-C12 saturated fatty acids, n-6 unsaturated fatty acids and n-9 unsaturated fatty acids One or more of them, the mass ratio of dispersant to gold in the reaction system is (0.05-0.2): 1;

[0050] (3) Add the aqueous solution of the reducing agent to the solution obtained in step (2), and stir at a speed of 400-500r / min until the reaction is complete, wherein the mass ratio of the reducing agent to gold in the reaction system is (2-5 ):1;

[0051] (4) Washing and drying the reaction product of step (3), the washing includes washing with lye, thereby preparing the micron-sized spherical hollow gold powder of the present invention. ...

Embodiment 1

[0087] Put 10g of sponge gold with a purity ≥ 99.9% in a 500mL beaker, add 40mL of prepared aqua regia in four times and heat to completely dissolve the pure gold, then add 10mL of concentrated hydrochloric acid to catch the nitrate, and then add deionized water to prepare 20mL concentration is the chloroauric acid solution of 0.5g gold / mL;

[0088] Dissolve 50 g of sodium sulfite completely with 200 mL of deionized water to obtain a sodium sulfite solution;

[0089] Dissolve 1.2g of oleic acid in 6g of absolute ethanol and set aside completely to obtain an oleic acid solution;

[0090] Dissolve 7g of sodium hydroxide with 70mL of deionized water to obtain a 100g / L sodium hydroxide solution;

[0091] Under the stirring condition of 180r / min, slowly pour 20mL sodium hydroxide solution into the 20mL chloroauric acid solution prepared above to adjust the pH value to 4~5. Pour all the solution into the gold-containing solution, stir for 10 minutes; then adjust the speed to 400r / ...

Embodiment 2

[0094] Put 10g of sponge gold with a purity ≥ 99.9% in a 500mL beaker, add 40mL of prepared aqua regia in four times and heat to completely dissolve the pure gold, then add 10mL of concentrated hydrochloric acid to catch the nitrate, and then add deionized water to prepare 20mL concentration is the chloroauric acid solution of 0.5g gold / mL;

[0095] Dissolve 25g of ascorbic acid completely with 125mL of deionized water to obtain ascorbic acid solution;

[0096] Dissolve 0.5g of octanoic acid in 2.5g of absolute ethanol and set aside completely to obtain octanoic acid solution;

[0097] Dissolve 7g of sodium hydroxide with 70mL of deionized water to obtain a 100g / L sodium hydroxide solution;

[0098] Under the stirring condition of 150r / min, slowly pour 20mL sodium hydroxide solution into the 20mL chloroauric acid solution prepared above to adjust the pH value to 4~5. Pour it all into the gold-containing solution, stir for 10 minutes; then adjust the speed to 400r / min, add al...

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Abstract

The invention provides micron-sized spherical hollow gold powder and a preparation method therefore. The preparation method for the micron-sized spherical hollow gold powder comprises: (1) adjusting the pH value of chloroauric acid solution to 4-5; (2) adding alcohol solution of dispersant to the solution obtained in step (1) for uniform stirring, wherein the dispersant is selected from one or more of C6-C12 saturated fatty acid, n-6 unsaturated fatty acid and n-9 unsaturated fatty acid; (3) adding water solution of a reducing agent to the solution obtained in step (2), and stirring at a rotation speed of 400-500 r / min to completely react; and (4) cleaning and drying a reaction product in step (3). The gold powder prepared in the invention has a particle size of 0.8-3.5 microns, and is excellent in dispersibility, free of agglomeration, excellent in infiltration with a carrier and suitable for electronic paste.

Description

technical field [0001] The invention belongs to the field of metal powder preparation, and in particular relates to a micron-sized spherical hollow gold powder and a preparation method thereof. Background technique [0002] Gold has high chemical stability, and its thermal conductivity and electrical conductivity are second only to silver and copper. After sintering in air, gold paste made of it can form a conductor with excellent electrical conductivity. It not only has excellent Weldability, but also excellent thermocompression welding performance and corrosion resistance, usually used in places requiring high reliability and high stability, such as aerospace, military engineering, medical equipment, computers and satellite communications and other fields. [0003] Most of the gold powders currently used in gold pastes are spherical, or flakes. Among them, due to the large shrinkage of high-temperature sintering, the flake gold powder is generally not used in thick-film g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/00B22F9/24
CPCB22F9/24B22F1/0655
Inventor 王要东雷莉君陆冬梅孙社稷张建益王雒瑶
Owner 西安宏星电子浆料科技股份有限公司
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