CN111230353B - Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste - Google Patents

Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste Download PDF

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Publication number
CN111230353B
CN111230353B CN202010061699.8A CN202010061699A CN111230353B CN 111230353 B CN111230353 B CN 111230353B CN 202010061699 A CN202010061699 A CN 202010061699A CN 111230353 B CN111230353 B CN 111230353B
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nano
silver
mixture
sno
tin oxide
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CN111230353A (en
Inventor
陈静
刘盼
张靖
叶怀宇
张国旗
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Southwest University of Science and Technology
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Shenzhen Third Generation Semiconductor Research Institute
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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
    • B23K35/02—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
    • 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
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • 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
    • B23K2101/00—Articles made by soldering, welding or cutting
    • B23K2101/36—Electric or electronic devices
    • 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
    • B23K2101/00—Articles made by soldering, welding or cutting
    • B23K2101/36—Electric or electronic devices
    • B23K2101/40—Semiconductor devices

Abstract

The invention provides nano Ag-SnO for improving silver electromigration2The preparation method and the application of the soldering paste comprise the following preparation steps: s1, fully mixing tin oxide particles with a diluent to obtain a first mixture; s2, mixing the nano silver particles with a diluent, an adhesive and a surfactant to obtain a second mixture; s3, adding the first mixture into the second mixture, uniformly stirring, and centrifuging to obtain Ag-SnO2And (4) nano soldering paste. The oxygen partial pressure of the nano-silver interconnection material is changed by adding tin oxide, so that the generation of an electromigration phenomenon is reduced; ag formed by silver and tin atoms3Sn retards silver electromigration, thereby extending the lifetime of the electronic package interconnect material; the invention has simple process flow and low cost, and is suitable for industrial application.

Description

Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste
Technical Field
The invention relates to the field of advanced materials for electronic packaging chip interconnection, in particular to nano Ag-SnO for improving silver electromigration2A preparation method and application of the solder paste.
Background
With the rapid development of electronic science and technology, the performance requirements of people on electronic power devices are continuously improved. Wide bandgap semiconductor power chips such as silicon carbide (SiC) and gallium nitride (GaN) have evolved rapidly due to their advantages in high temperature high power or high heat dissipation applications. The high temperature conditions (above 250 ℃) under which they operate present a significant challenge to conventional packaging processes. Therefore, the research on the chip interconnection level package of the wide bandgap semiconductor power device is particularly important for its application at high temperature, and it is necessary to research and develop a chip interconnection material with good thermal, electrical, mechanical properties and high temperature reliability. In recent years, the proposal for sintering and packaging electronic chips by using nano metal has attracted wide attention at home and abroad, and the basic principle is to realize low-temperature and low-pressure sintering and packaging by using the characteristics of high surface energy and low melting point of nano metal particles. Based on the principle, the low-temperature sintering connection of the nano silver paste becomes a research hotspot in recent years. The nano silver paste sintering package has the characteristics of low-temperature and low-pressure sintering, the sintering layer can theoretically resist the high temperature below 960 ℃, and meanwhile, the silver has good electric conduction, heat conduction and ductility, so that the nano silver paste sintering package can be used for packaging high-temperature electronic products. However, the development of the nano silver solder paste is influenced by the electromigration phenomenon generated in the using process of the nano silver solder paste.
It was found that the partial pressure of oxygen in the nanosilver solder paste has a large influence on the electromigration of silver. Tin metal material is the most widely used material, however, with the development of the electronic industry and the continuous development of high-temperature chips, the development is limited by the lower service temperature of tin, and tin oxide is a stable conductive material and is used as an industrial doping material. The technical problems solved by the invention are as follows: the phenomenon of package failure caused by current leakage caused by electromigration in the use process of the nano-silver soldering paste is reduced.
Disclosure of Invention
The invention provides nano Ag-SnO for improving silver electromigration, aiming at solving the problems of high cost of nano silver prepared by the existing method and service temperature of a soldering paste sintering material2The preparation method of the soldering paste comprises the following preparation steps:
s1, mixing tin oxide particles with a diluent to obtain a first mixture;
s2, mixing the nano silver particles with a diluent, an adhesive and a surfactant to obtain a second mixture;
s3, adding the first mixture into the second mixture, uniformly stirring, and centrifuging to obtain Ag-SnO2Nano solder paste;
the mass ratio of the tin oxide particles to the diluent is 1: 1-2.5;
Ag-SnO2the mass percent of silver in the nano soldering paste is 98.90-67.92%;
the mass percentage of the first mixture in the total mass of the first mixture and the second mixture is 0.09-39.76%.
The conductivity of tin oxide is increased along with the increase of the temperature, the tin oxide presents N-type semiconductor property due to oxygen vacancy defects in the crystal, the temperature is increased, the moving speed of carriers is accelerated, and therefore the conductivity is increased, the thermal conductivity is good, the chemical property is stable, and the tin oxide can be used as a novel high-temperature chip interconnection material.
Preferably, the particle size of the tin oxide is 20-100 nm, and the particle size of the nano silver soldering paste is 20-100 nm.
The particle diameters of the nano silver soldering paste and the nano tin dioxide are kept similar, which is beneficial to the embodiment of the performance of the mixture; the electromigration of silver is closely related to the partial pressure of oxygen, e.g. Ag-SnO2The tin oxide in the silver oxide has a function of slowing down the electrochemical migration of silver, and can effectively improve the electromigration of the silver.
Preferably, the diluent is selected from one or a mixture of more of terpineol, ethanol, glycol and isobutanol.
The thinner is added to adjust the viscosity of the solder paste so as to facilitate nano Ag-SnO2And coating and printing the solder paste.
Preferably, the binder is selected from polyvinyl alcohol, polyvinyl butyral.
Preferably, the surfactant is a fatty acid glyceride.
Preferably, the stirring condition in the S3 is 1000-2000 r/min of rotation speed and 30-60S of time.
It has the functions of stirring and dispersing high viscosity material and helping dispersing nano particle to prepare Ag-SnO2A solder paste.
A sintering method of the nano tin oxide and silver composite soldering paste prepared by the method comprises the following steps:
s1, coating the nano tin oxide and silver composite soldering paste on a substrate;
s2, chip bonding;
and S3, sintering, cooling and finishing the preparation of the device.
The nano tin oxide silver composite solder paste can be applied to the technical fields of automobile electronics, power electronics, IGBT, wide bandgap semiconductor packaging and the like.
Silver oxide generated in the sintering process of the nano-silver solder paste can be decomposed at 250 ℃ to generate oxygen so as to intensify silver electromigration, and the sintered Ag-doped silver paste is prepared by the inventionSnO2The tin oxide in the nano soldering paste can influence the oxygen partial pressure in the high-temperature service electronic packaging interconnection material, so that the content of oxygen required by silver ionization is reduced, the content of silver ions is reduced, and the electromigration of silver is effectively improved. Simultaneously, Ag reacts with Sn atoms to form Ag3Sn is reduced and Ag3Sn acts to hinder silver electromigration.
Preferably, the thickness of the nano tin oxide silver composite solder paste in S1 is 25-35 μm.
Preferably, the sintering condition of S3 is pressure of 10-20 MPa; the sintering process is as follows: rapidly heating to 160 deg.C, and maintaining the constant temperature for 15min-30 min; rapidly heating to 180 deg.C, and maintaining the constant temperature for 15min-30 min; quickly heating to 230-250 deg.C, and holding the temperature for 50-80 min.
If the chip is small-sized, no pressurization is needed, and no inert gas protection is needed.
The beneficial effects of the invention at least comprise:
1. the oxygen partial pressure of the nano-silver interconnection material is changed by adding tin oxide, so that the generation of an electromigration phenomenon is reduced.
2. Ag formed by silver and tin atoms3Sn retards silver electromigration, thereby extending the useful life of the electronic package interconnect material.
3. The invention has simple process flow and low cost, and is suitable for industrial application.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
Example 1
S1, fully mixing 25 nm-sized tin oxide particles with a diluent to obtain a first mixture, wherein the mass percentage of the mixture of the tin oxide and the diluent is 6%; s2, mixing the nano silver particles with the size of 25nm with a diluent (terpineol and ethanol), an adhesive (polyvinyl alcohol) and the surfaceMixing the active agents (fatty glyceride) to obtain a second mixed solution; s3, adding the first mixture into a second mixed solution, wherein the mass percent of the first mixture in the total mass of the first mixture and the second mixture is 6%, uniformly stirring at a rotating speed of 1500r/min, and centrifuging to obtain Ag-SnO2The nano solder paste has the conductivity of 125 +/-10W/mK.
Example 2
S1, fully mixing 25 nm-sized tin oxide particles with a diluent to obtain a first mixture, wherein the mass percentage of the mixture of the tin oxide and the diluent is 6%; s2, mixing nano silver particles with the size of 25nm with diluents (terpineol and ethanol), adhesives (polyvinyl alcohol) and surfactants (fatty glyceride) to obtain a second mixed solution; s3, adding the first mixture into a second mixed solution, wherein the mass percent of the first mixture in the total mass of the first mixture and the second mixture is 15%, uniformly stirring at a rotating speed of 1500r/min, and centrifuging to obtain Ag-SnO2The thermal conductivity of the nano-soldering paste is 125 +/-10W/mK.
Example 3
S1, fully mixing 25 nm-sized tin oxide particles with a diluent to obtain a first mixture, wherein the mass percentage of the mixture of the tin oxide and the diluent is 6%; s2, mixing nano silver particles with the size of 25nm with diluents (terpineol and ethanol), adhesives (polyvinyl alcohol) and surfactants (fatty glyceride) to obtain a second mixed solution; s3, adding the first mixture into a second mixed solution, wherein the mass percent of the first mixture in the total mass of the first mixture and the second mixture is 30%, uniformly stirring at a rotating speed of 1500r/min, and centrifuging to obtain Ag-SnO2The thermal conductivity of the nano-soldering paste is 125 +/-10W/mK.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims (7)

1. Nano Ag-SnO for improving silver electromigration2The preparation method of the soldering paste is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1, mixing tin oxide particles with a diluent to obtain a first mixture;
s2, mixing the nano silver particles with a diluent, an adhesive and a surfactant to obtain a second mixture; the adhesive is selected from polyvinyl alcohol and polyvinyl butyral; the diluent is one or a mixture of more of ethylene glycol and isobutanol;
s3, adding the first mixture into the second mixture, uniformly stirring, and centrifuging to obtain Ag-SnO2Nano solder paste;
the Ag-SnO2The tin oxide in the nano soldering paste can influence the oxygen partial pressure in the high-temperature service electronic packaging interconnection material, so that the oxygen content required by silver ionization is reduced, the silver ion content is reduced, and the silver electromigration is effectively improved; meanwhile, the stirring ensures that the particles added into the second mixture from the first mixture are uniformly mixed so as to react at high temperature in the sintering process to generate Ag3Sn and hinders the effect of silver electromigration;
the mass ratio of the tin oxide particles to the diluent is 1: 1-2.5;
the Ag-SnO2The mass percent of silver in the nano soldering paste is 98.90-67.92%;
the mass percentage of the first mixture in the total mass of the first mixture and the second mixture is 0.09-39.76%.
2. The nano Ag-SnO with improved silver electromigration improvement effect as claimed in claim 12The preparation method of the soldering paste is characterized by comprising the following steps: the size of the tin oxide particles is 20-100 nm, and the Ag-SnO2The particle size of the nano soldering paste is 20-100 nm.
3. The nano Ag-SnO with improved silver electromigration improvement effect as claimed in claim 12The preparation method of the soldering paste is characterized by comprising the following steps: the surfactant is fatty acidA glyceride.
4. The nano Ag-SnO with improved silver electromigration improvement effect as claimed in claim 12The preparation method of the soldering paste is characterized by comprising the following steps: and in the S3, the stirring condition is 1000-2000 r/min of rotation speed and 30-60S of time.
5. A sintering method of nano tin oxide silver composite solder paste prepared by the method of any one of claims 1 to 4, characterized in that: the method comprises the following steps:
s1, coating the nano tin oxide and silver composite soldering paste on a substrate;
s2, chip bonding;
and S3, sintering, cooling and finishing the preparation of the device.
6. The sintering method according to claim 5, wherein: the thickness of the nano tin oxide silver composite soldering paste in the S1 is 25-35 mu m.
7. The sintering method according to claim 5, wherein: the sintering condition of S3 is that the pressure is 10-20 MPa; the sintering process is as follows: rapidly heating to 160 deg.C, and maintaining the constant temperature for 15min-30 min; rapidly heating to 180 deg.C, and maintaining the constant temperature for 15min-30 min; quickly heating to 230-250 deg.C, and holding the temperature for 50-80 min.
CN202010061699.8A 2020-01-19 2020-01-19 Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste Active CN111230353B (en)

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CN112475663B (en) * 2020-11-17 2022-05-10 云南锡业锡材有限公司 Preparation method of lead-free composite soldering paste with high spreading rate

Citations (6)

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Publication number Priority date Publication date Assignee Title
CN101923929A (en) * 2009-06-10 2010-12-22 E.I.内穆尔杜邦公司 Chip resistor front electrode and backplate
CN104737238A (en) * 2012-10-19 2015-06-24 纳美仕有限公司 Electroconductive paste
CN106271200A (en) * 2016-08-23 2017-01-04 天津大学 The preparation method of the Ag Pd nano-solder paste that resistance to Ag migrates under a kind of hot environment
CN109277723A (en) * 2018-10-06 2019-01-29 天津大学 The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste
CN109277722A (en) * 2018-10-06 2019-01-29 天津大学 A kind of preparation method for the Ag-Si nano-solder paste improving silver-colored electrochemical migration
CN109822259A (en) * 2019-03-26 2019-05-31 深圳市聚威新材科技有限公司 A kind of soldering paste

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101923929A (en) * 2009-06-10 2010-12-22 E.I.内穆尔杜邦公司 Chip resistor front electrode and backplate
CN104737238A (en) * 2012-10-19 2015-06-24 纳美仕有限公司 Electroconductive paste
CN106271200A (en) * 2016-08-23 2017-01-04 天津大学 The preparation method of the Ag Pd nano-solder paste that resistance to Ag migrates under a kind of hot environment
CN109277723A (en) * 2018-10-06 2019-01-29 天津大学 The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste
CN109277722A (en) * 2018-10-06 2019-01-29 天津大学 A kind of preparation method for the Ag-Si nano-solder paste improving silver-colored electrochemical migration
CN109822259A (en) * 2019-03-26 2019-05-31 深圳市聚威新材科技有限公司 A kind of soldering paste

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Effective date of registration: 20230327

Address after: No. 1088, Xueyuan Avenue, Taoyuan Street, Nanshan District, Shenzhen City, Guangdong Province

Patentee after: SOUTH University OF SCIENCE AND TECHNOLOGY OF CHINA

Address before: Taizhou building, No. 1088, Xueyuan Avenue, Xili University Town, Nanshan District, Shenzhen City, Guangdong Province

Patentee before: SHENZHEN THIRD GENERATION SEMICONDUCTOR Research Institute