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Nano silver copper wrapped welding flux preparing method based on phonochemistry

A nano-silver, sonochemical technology, applied in welding equipment, nanotechnology, welding/cutting media/materials, etc., can solve the problems of high cost of nano-silver paste, electromigration of nano-copper paste, shortening reaction time, etc., and achieve high service life Effects of temperature, increased activity and energy, and availability of raw materials

Active Publication Date: 2020-09-04
HARBIN INSTITUTE OF TECHNOLOGY SHENZHEN (INSTITUTE OF SCIENCE AND TECHNOLOGY INNOVATION HARBIN INSTITUTE OF TECHNOLOGY SHENZHEN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the above technical problems, the present invention discloses a method for preparing nano-silver clad copper solder based on sonochemistry, utilizing the special effect of ultrasonic waves in the liquid phase, While ensuring stable performance, the reaction time is greatly shortened, and the process is simple and efficient to prepare, so as to obtain nano-level silver-coated copper solder paste with the characteristics of low-temperature connection and high-temperature service, which solves the high cost of nano-silver paste in industrial applications. Poor reliability problems caused by serious migration and instability of nano-copper paste

Method used

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  • Nano silver copper wrapped welding flux preparing method based on phonochemistry
  • Nano silver copper wrapped welding flux preparing method based on phonochemistry
  • Nano silver copper wrapped welding flux preparing method based on phonochemistry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Weigh 10 g of copper sulfate pentahydrate powder and add it to 100 ml of ethylene glycol, heat to 70°C, stir for 15 min until completely dissolved to obtain solution A. In addition, weigh 8g of sodium hypophosphite powder, add 5g of polyvinylpyrrolidone into 200ml of ethylene glycol, heat to 70°C, stir for 20 minutes and wait for complete dissolution to obtain solution B.

[0056] (2) Add the freshly prepared solution A to the freshly prepared solution B, and apply a horn-type (horn) pulsed ultrasonic wave (power 200 W, pulse ratio 2 s-2 s) acting straight down, and heat to 70 ℃, react for 15 min, and the copper nanoparticle dispersion can be obtained.

[0057] (3) Cool the copper nanoparticle dispersion obtained in step (2) to room temperature and centrifuge (5000 rpm, 15 min), and use a mixed solution of absolute ethanol: deionized water at a volume ratio of 3:1 Wash 3 times.

[0058] (4) Weigh 2 g of Cu nanoparticles obtained in step (3) and 2 g of sodium citra...

Embodiment 2

[0064] (1) Weigh 10 g of copper sulfate pentahydrate powder and add it to 100 ml of ethylene glycol, heat to 70°C, stir for 15 min until completely dissolved to obtain solution A. In addition, weigh 8g of sodium hypophosphite powder, add 5g of polyvinylpyrrolidone into 200ml of ethylene glycol, heat to 70°C, stir for 20 minutes and wait for complete dissolution to obtain solution B.

[0065] (2) Add the freshly prepared solution A to the freshly prepared solution B, and apply a horn-type (horn) pulsed ultrasonic wave (400 W, pulse ratio of 2 s-2 s) acting directly downward, and heat to 70 °C, After 15 min of reaction, the copper nanoparticle dispersion can be obtained.

[0066] (3) Cool the copper nanoparticle dispersion obtained in step (2) to room temperature and centrifuge (5000 rpm, 15 min), and use a mixed solution of absolute ethanol: deionized water at a volume ratio of 3:1 Wash 3 times.

[0067] (4) Weigh 2 g of Cu nanoparticles obtained in step (3) and 2 g of sodium...

Embodiment 3

[0072] (1) Weigh 10 g of copper sulfate pentahydrate powder and add it to 100 ml of ethylene glycol, heat to 70°C, stir for 15 min until completely dissolved to obtain solution A. In addition, weigh 8g of sodium hypophosphite powder, add 5g of polyvinylpyrrolidone into 200ml of ethylene glycol, heat to 70°C, stir for 20 minutes and wait for complete dissolution to obtain solution B.

[0073] (2) Add the freshly prepared solution A to the freshly prepared solution B, and apply a horn-type (horn) pulsed ultrasonic wave (600 W, pulse ratio 4 s-2 s) acting straight down, and heat to 70 °C, After 15 min of reaction, the copper nanoparticle dispersion can be obtained.

[0074](3) Cool the copper nanoparticle dispersion obtained in step (2) to room temperature and centrifuge (5000 rpm, 15 min), and use a mixed solution of absolute ethanol: deionized water at a volume ratio of 3:1 Wash 3 times.

[0075] (4) Weigh 2 g of Cu nanoparticles obtained in step (3) and 2 g of sodium citrate...

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Abstract

The invention provides a nano silver copper wrapped welding flux preparing method based on phonochemistry. The preparing method comprises the following steps that a copper salt organic solvent solution and a sodium phosphite and protective agent organic solvent solution are mixed, horn type pulse ultrasonic waves straight downwards are applied into the solution, copper nano particle dispersion liquid is obtained through the heating reaction, and Cu nano particles are obtained through cooling, centrifuging and washing; the Cu nano particles and a reducing agent are added in deionized water to be evenly mixed, a silver salt solution is added for the reaction at 30-50 DEG C, silver copper wrapped nano particle dispersion liquid is obtained, the silver copper wrapped nano particle dispersion liquid is centrifuged and washed, and silver copper wrapped nano particles are obtained; and the silver copper wrapped nano particles and a welding paste organic solvent are evenly mixed, and silver copper wrapped nano particle welding paste is obtained. The silver copper wrapped nano particle welding flux prepared through the technical scheme is high in reliability and has the characteristics of low-temperature connection and high-temperature service, protective gas is not needed in the preparing process, the technology is simple, and green and environment protection are achieved.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method of nanometer silver-coated copper solder based on sonochemistry. Background technique [0002] Since the beginning of the new century, the trend of light weight and miniaturization of electronic products has become more and more obvious, and nano-conductive particles, as interconnect materials in microelectronic products, are very important components. When the nano-conductive particles are made into a conductive paste by means of dispersion, it meets the requirements of bonding materials for micro-nano connection and other processes in high-power devices. At the same time, with the continuous development of the semiconductor industry and entering the post-Moore era, the concept of combining silicon-based and non-silicon-based technologies has been proposed, which also puts forward higher requirements for packaging materials, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/02B22F1/00B23K35/36B23K35/362B82Y40/00
CPCB22F9/24B23K35/3612B23K35/362B82Y40/00B22F1/07B22F1/054B22F1/107B22F1/17
Inventor 计红军张文武修子进马秋晨曹依琛潘浩张琳李明雨
Owner HARBIN INSTITUTE OF TECHNOLOGY SHENZHEN (INSTITUTE OF SCIENCE AND TECHNOLOGY INNOVATION HARBIN INSTITUTE OF TECHNOLOGY SHENZHEN)
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