CN109277723B - Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste - Google Patents

Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste Download PDF

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CN109277723B
CN109277723B CN201811164526.8A CN201811164526A CN109277723B CN 109277723 B CN109277723 B CN 109277723B CN 201811164526 A CN201811164526 A CN 201811164526A CN 109277723 B CN109277723 B CN 109277723B
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nano
sio
silver
soldering paste
solder paste
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CN109277723A (en
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梅云辉
李丹
李欣
陆国权
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Tianjin University
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Tianjin University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3006—Ag as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries

Abstract

The invention relates to Ag-SiO resisting silver electromigration in a high-temperature environment2A preparation method of nano soldering paste; mixing silicon dioxide powder with the average particle size of 20-100 nm and a diluent under the assistance of ultrasonic water bathCombining; adding the mixture into nano-silver soldering paste with the average particle size of 50-500 nm, and uniformly stirring and mixing to obtain Ag-SiO2Nano solder paste; the thinner is added to adjust the viscosity of the solder paste so as to facilitate the nano Ag-SiO2And coating and printing the solder paste. The prepared Ag-SiO2The nano solder paste and the commercially available nano silver solder paste are sintered at a heating rate of 5 ℃/min at 280 ℃, are cooled in a furnace after heat preservation for 30min, and then are subjected to electromigration experiments at a high temperature of 400 ℃ and an electric field strength of 400V/mm. The results demonstrate that Ag-SiO2The failure life of the nano-solder paste is at least improved by 3.60 times compared with that of the nano-silver solder paste.

Description

Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste
Technical Field
The invention relates to Ag-SiO for improving silver electromigration phenomenon in high-temperature environment2A preparation method of nano soldering paste, which is used for connecting electronic devices, belongs to the field of advanced material preparation and electronic device packaging.
Background
In recent years, the nano silver solder paste replaces the traditional method of providing sintering driving force by depending on mechanical pressure, realizes sintering under the conditions of no pressure and low temperature, obtains reliable lead-free environment-friendly connection, and is widely applied to wide-bandgap semiconductor high-temperature power chips (such as SiC and GaN). In addition, the nano Ag soldering paste has the advantages of good electrical conductivity, good thermal conductivity, excellent fatigue resistance, suitability for high-temperature high-power and high-density packaging, good machinability, greenness, no lead, low process temperature and the like, and gradually replaces the traditional tin-lead solder to become a preferred interconnection material for high-temperature application of high-power electronic devices along with the development of the power electronic industry.
Silver, however, is a metal that migrates very readily and at a fast rate, especially in high temperature or humid environments. This is because the activation energy required for anodic dissolution is extremely low compared to other metals when an electric field is present in a high-temperature humid environment. Silver migration can alter dielectric properties, reduce insulation resistance, cause silver "bridges" to form, short circuit between electrodes, affect reliability and contribute to device failure. As electronic components move toward miniaturization, the risk of device failure due to electrochemical migration of silver increases with decreasing conductor spacing in electronic packages. The effect of silver electromigration on its performance in electronic packaging must therefore be of our concern. How to improve or inhibit the electromigration of the silver and increase the failure life of the electronic component has important significance.
The electromigration of silver is closely related to the partial pressure of oxygen, e.g. Ag-SiO2The silicon dioxide in the silver oxide has a function of slowing down the electrochemical migration of the silver, and can effectively improve the electromigration of the silver. Therefore, it is necessary to develop a conductive paste of silver and silicon dioxide.
Disclosure of Invention
Aiming at the problem of silver electromigration when nano silver soldering paste is connected with a high-temperature power chip in electronic packaging, the invention aims at the improved part of the connecting material, so that the electronic component can meet the requirement of prolonging the failure life under the action of higher temperature and electric field.
The technical scheme of the invention is as follows:
Ag-SiO resistant to silver electromigration in high-temperature environment2The preparation method of the nano soldering paste comprises the following steps: fully mixing silicon dioxide powder with the average particle size of 20-100 nm and a diluent under the assistance of ultrasonic water bath; adding the mixture into nano-silver soldering paste with the average particle size of 50-500 nm, and uniformly stirring and mixing to obtain Ag-SiO2Nano solder paste; the thinner is added to adjust the viscosity of the solder paste so as to facilitate the nano Ag-SiO2And coating and printing the solder paste.
The Ag-SiO2The mass percent of the silver soldering paste in the nano soldering paste is 99.82-68.22%, and the mass percent of the corresponding mixture of the silicon dioxide powder and the thinner is 0.18-31.78%.
The mass ratio of the silicon dioxide powder to the diluent is 1: 1-2.
The diluent is an alcohol solvent, such as terpineol or ethanol.
And mixing for 15-45 min with the assistance of ultrasonic water bath to fully mix the silicon dioxide powder and the diluent.
At a rotation speed of 1000-2000 r/minStirring for 30-60 s under a high-efficiency stirrer to prepare Ag-SiO2And (4) nano soldering paste. The rotating speed is low, and the stirring time is long; the rotating speed is high, and the stirring time is short. It can stir and disperse high viscosity material simultaneously, and can help the dispersion of nano particles to prepare Ag-SiO2A solder paste.
The sintered nano Ag-SiO2The silicon dioxide in the nano soldering paste has a slowing effect on the electrochemical migration of silver, and the migration of the silver can be effectively improved. Heating Ag-SiO at a rate of 5 deg.C/min2The nano soldering paste and the commercially obtained nano silver soldering paste are sintered at 280 ℃, are kept warm for 30min, are cooled in a furnace (aiming at the problems that the drying of organic matters of a large-area chip bonding sample and the ablation of a binder are slow, and after a plurality of tests, the heating rate of a sintering heating curve is 5 ℃/min, the final temperature is 280 ℃, and the heat preservation is 30min), are subjected to an electromigration test at the high temperature of 400 ℃ and the electric field intensity of 400V/mm, and the results show that the Ag-SiO soldering paste is subjected to the electromigration test at the2The nano-soldering paste greatly prolongs the service life of failure, and compared with nano-silver soldering paste, the Ag-SiO2The failure life of the nano soldering paste is improved by at least 3.60 times; and Ag-SiO2The nano soldering paste has the advantages of simple preparation process, high preparation efficiency and low cost.
Ag-SiO2The nano soldering paste can obviously improve or inhibit silver migration when being connected with a high-temperature power chip, increase the failure life of electronic components and meet the use requirement of electronic packaging.
Embodiments include, but are not limited to, heating stations, ovens, and the like.
The invention has the following effects:
(1) prepared Ag-SiO2The failure life of the nano-solder paste is at least improved by 3.60 times compared with that of the nano-silver solder paste.
(2) Nano Ag-SiO2The bonding strength of the soldering paste connecting chip can stably reach about 27 MPa.
(3) The invention has the advantages of simple preparation process, high efficiency, good stability and low cost.
Drawings
FIG. 1: after mixing in the ratio of example 1, Ag-SiO2Electrochemical migration of nano-solder paste and nano-silver solder pasteAnd (5) a graph of the leakage current in the process of testing along with time. The time when the leakage current value reaches 1mA is specified as the failure life, the average failure life of the nano-silver soldering paste is about 286min, and Ag-SiO2The average failure life of the nano-solder paste is 1029min, and the failure life of the nano-solder paste is at least 3.60 times longer than that of the nano-silver solder paste.
Detailed Description
Mixing silicon dioxide powder with the average particle size of 20-100 nm and a diluent under the assistance of ultrasonic water bath, adding the mixture into nano silver soldering paste with the average particle size of 50-500 nm, and uniformly stirring and mixing to obtain Ag-SiO2A nano-class soldering paste for preparing Ag-SiO particles at ordinary temp2Method for preparing nano soldering paste and prepared Ag-SiO2The nano-soldering paste has the advantages of excellent performance, simple process, low cost and good stability. The method comprises the following specific steps:
(a) preparation of a mixture of silica powder and diluent: mixing silicon dioxide powder with the average particle size of 20-100 nm and a diluent (terpineol or ethanol) for 15-45 min with the assistance of an ultrasonic water bath;
(b) preparing a mixture of silver, silica powder and diluent: adding the mixture of the silicon dioxide powder and the diluent into nano-silver soldering paste with the average particle size of 50-500 nm to obtain a mixture of silver, the silicon dioxide powder and the diluent;
(c) stirring: stirring the mixture of the silver powder, the silicon dioxide powder and the diluent obtained in the step (b) for 30-60 s by using a high-efficiency stirrer with the rotating speed of 1000-2000 r/min to obtain Ag-SiO2And (4) nano soldering paste.
Example 1
(a) Mixing silicon dioxide powder with the average particle size of 20-100 nm and terpineol serving as a diluent for 30min with the aid of an ultrasonic water bath, wherein the mass of the silicon dioxide powder is 0.1g, and the mass of the terpineol is 0.1 g;
(b) adding a mixture of silicon dioxide powder and terpineol serving as a diluent into nano silver soldering paste with the average particle size of 50-500 nm, wherein the mass of the silver soldering paste is 113.52g, and obtaining a mixture of silver, silicon dioxide powder and terpineol;
(c) stirring the mixture of the silver powder, the silicon dioxide powder and the terpineol obtained in the step (b) for 60s by a high-efficiency stirrer with the rotating speed of 2000r/min to prepare the Ag-SiO2And (4) nano soldering paste.
Example 2
(a) Mixing silicon dioxide powder with the average particle size of 20-100 nm and terpineol serving as a diluent for 15min with the aid of an ultrasonic water bath, wherein the mass of the silicon dioxide powder is 5g, and the mass of the terpineol is 7.5 g;
(b) adding a mixture of silicon dioxide powder and terpineol serving as a diluent into nano silver soldering paste with the average particle size of 50-500 nm, wherein the mass of the silver soldering paste is 107.95g, and obtaining a mixture of silver, silicon dioxide powder and terpineol;
(c) stirring the mixture of the silver powder, the silicon dioxide powder and the terpineol obtained in the step (b) for 45s by a high-efficiency stirrer with the rotating speed of 1500 r/min to obtain Ag-SiO2And (4) nano soldering paste.
Example 3
(a) Mixing silicon dioxide powder with the average particle size of 20-100 nm and diluent ethanol for 45min under the assistance of ultrasonic water bath, wherein the mass of the silicon dioxide powder is 15g, and the mass of the ethanol is 30 g;
(b) adding a mixture of silicon dioxide powder and diluent ethanol into nano silver soldering paste with the average particle size of 50-500 nm, wherein the mass of the silver soldering paste is 96.59g, and obtaining a mixture of silver, silicon dioxide powder and ethanol;
(c) stirring the mixture of the silver, the silicon dioxide powder and the ethanol obtained in the step (b) for 30s by a high-efficiency stirrer with the rotating speed of 1000r/min to prepare the Ag-SiO2And (4) nano soldering paste.
Ag-SiO prepared by the embodiment of the invention2The nano solder paste and the commercially available nano silver solder paste are sintered at a heating rate of 5 ℃/min at 280 ℃, are cooled in a furnace after heat preservation for 30min, and then are subjected to electromigration experiments at a high temperature of 400 ℃ and an electric field strength of 400V/mm. The results demonstrate that Ag-SiO2The failure life of the nano-silver soldering paste is at least improved by 3.60 times compared with that of the nano-silver soldering paste.
While all methods disclosed and claimed herein have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and subcombinations of the methods and techniques described herein may be made to achieve the final product without departing from the spirit, scope, or scope of the invention. Ag-SiO2The nano soldering paste can obviously improve or inhibit the electromigration of silver when being connected with a high-temperature power chip, increase the failure life of electronic components and meet the use requirement of electronic packaging.

Claims (3)

1. Ag-SiO resistant to silver electromigration in high-temperature environment2The preparation method of the nanometer soldering paste is characterized in that silicon dioxide powder with the average particle size of 20-100 nm and an alcohol diluent are mixed under the assistance of ultrasonic water bath; then adding the mixture into nano silver soldering paste with the average particle size of 50-500 nm, and uniformly stirring and mixing to obtain Ag-SiO2And (4) nano soldering paste.
2. The method according to claim 1, wherein said Ag-SiO is2The mass percentage of the silver soldering paste in the nano soldering paste is 99.82-68.22%.
3. The method according to claim 1, wherein the ratio of the mass of the silica powder to the mass of the diluent is 1:1 to 2.
CN201811164526.8A 2018-10-06 2018-10-06 Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste Active CN109277723B (en)

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CN111230353B (en) * 2020-01-19 2021-08-17 深圳第三代半导体研究院 Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste
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