CN109277723A - The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste - Google Patents
The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste Download PDFInfo
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- CN109277723A CN109277723A CN201811164526.8A CN201811164526A CN109277723A CN 109277723 A CN109277723 A CN 109277723A CN 201811164526 A CN201811164526 A CN 201811164526A CN 109277723 A CN109277723 A CN 109277723A
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- sio
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- solder paste
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- silver
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Classifications
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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 present invention relates to a kind of Ag-SiO of silver electromigration resistance under hot environment2The preparation method of nano-solder paste；The SiO 2 powder that average particle size particle size is 20~100nm is mixed under the assistance of ultrasonic water bath with diluent；It is added in the nano mattisolda that average particle size particle size is 50~500nm, and stirs by mixing obtained Ag-SiO2Nano-solder paste；Adding diluent is to adjust the viscosity of soldering paste in order to nanometer Ag-SiO2Coating, the printing of soldering paste.By Ag-SiO obtained2Nano-solder paste and commercially-available nano mattisolda are sintered at 280 DEG C with the rate of heat addition of 5 DEG C/min respectively, and furnace is cold after keeping the temperature 30min, and electromigration experiment is then carried out under 400 DEG C of hot conditions, 400V/mm electric field strength.As a result Ag-SiO is proved2The burn-out life of nano-solder paste at least improves 3.60 times compared to nano mattisolda.
Description
Technical field
The present invention relates to a kind of applied to the Ag-SiO for improving silver-colored ELECTROMIGRATION PHENOMENON in hot environment2The preparation of nano-solder paste
Method, the nano-solder paste are used for connection of electronic devices, belong to advanced material preparation and electronic component encapsulation field.
Background technique
In recent years, nanoscale nano mattisolda replaces tradition to provide the method for sintering driving force by mechanical pressure, real
Show without the sintering under pressure, low temperature and obtained reliable, leadless environment-friendly connection, has been widely used in wide band gap semiconducter high temperature power
Chip (such as SiC, GaN).Furthermore nanometer Ag soldering paste it is conductive it is good, thermal conductivity is good, anti-fatigue performance is excellent, be suitable for high temperature
It is high-power with high-density packages, machinability is good, the unleaded advantages such as low with technological temperature of green, with the hair of power electronics industry
Exhibition, gradually replacing conventional tin-lead solders becomes the preferred interconnection material of high-power electronic device high temperature application.
However silver is a kind of metal easily migrated, and migration rate is fast, especially in high temperature or wet environment.
This is because in the presence of having electric field, activation energy needed for opposite its anodic solution of other metals is extremely low under hot humid environment.
Silver migration can change dielectric properties, reduce insulation resistance, cause silver-colored " electric bridge " to be formed, make short circuit between electrodes, influence reliable
Property simultaneously promotes equipment failure.Develop with electronic component to trend toward miniaturization, the reduction of conductor spacing in Electronic Packaging, due to silver
Electrochemical migration and bring equipment failure risk will increase.Therefore the electromigration of silver is to its influence in Electronic Packaging
It must cause our concern.The electromigration for how improving or inhibiting silver increases the burn-out life of electronic component with important
Meaning.
The electromigration of silver and the partial pressure of oxygen are closely related, such as Ag-SiO2In silica to silver electrochemical migration
Have and slow down effect, can effectively improve the electromigration of silver.Therefore develop a kind of silver is highly desirable with silica electrocondution slurry.
Summary of the invention
Existing silver-colored problems of electromigration when connecting high temperature power chip the present invention be directed to nano mattisolda in Electronic Packaging,
The improvement part for aiming at connecting material, is able to satisfy electronic component under the action of higher temperature and electric field, the burn-out life
It is promoted.
Technical scheme is as follows:
The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste: it is by average particle size particle size
The SiO 2 powder and diluent of 20~100nm is sufficiently mixed under the assistance of ultrasonic water bath；Be mixed object be added to it is flat
In the nano mattisolda that equal particle size is 50~500nm, and stir by mixing obtained Ag-SiO2Nano-solder paste；Add
Diluent is added to be in order to adjust the viscosity of soldering paste in order to nanometer Ag-SiO2Coating, the printing of soldering paste.
The Ag-SiO2The mass percent of silver paste is 99.82%~68.22%, corresponding two in nano-solder paste
The mass percent of the mixture of silicon oxide powder and diluent is 0.18%~31.78%.
The quality of the SiO 2 powder and the mass ratio of diluent are 1:1~2.
The diluent is alcohols solvent, such as terpinol or ethyl alcohol.
15~45min is mixed under the assistance of ultrasonic water bath, and SiO 2 powder is enable to be sufficiently mixed with diluent.
In the case where revolving speed is the high-efficiency stirring instrument of 1000~2000r/min, Ag-SiO is made in 30~60s of stirring2Nano-solder paste.
Revolving speed is small, and mixing time is long；Revolving speed is big, and mixing time is short.Its effect is to carry out the stirring of heavy viscous material simultaneously and divide
It dissipates, nano particle dispersion can be helped to which Ag-SiO be made2Soldering paste.
Sintered nanometer Ag-the SiO of the present invention2Silica in nano-solder paste, which has the electrochemical migration of silver, slows down work
With, can effectively improve silver migration.With the rate of heat addition of 5 DEG C/min by Ag-SiO2Nano-solder paste and commercially-available nano silver
Soldering paste is sintered at 280 DEG C respectively, and furnace is cold (for the baking of some large-area chips bonding sample organic matters after keeping the temperature 30min
Dry and binder ablation is slower, and by test of many times, the rate of heat addition for being sintered heating curves is 5 DEG C/min, and final temperature is
280 DEG C, keep the temperature 30min), electromigration experiment is then carried out under 400 DEG C of high temperature, 400V/mm electric field strength, the results showed that Ag-
SiO2Nano-solder paste substantially increases the burn-out life, compared with nano mattisolda, Ag-SiO2The burn-out life of nano-solder paste is at least
Improve 3.60 times；And Ag-SiO2Nano-solder paste preparation process is simple, and preparation efficiency is high, at low cost.
Ag-SiO2Nano-solder paste can be obviously improved when connecting high temperature power chip or inhibit the migration of silver, increase electronics
The burn-out life of component meets Electronic Packaging requirement.
Embodiment includes but is not limited to the heating equipments such as warm table, baking oven.
Effect of the invention:
(1) Ag-SiO prepared2Nano-solder paste, burn-out life at least improve 3.60 times compared to nano mattisolda.
(2) nanometer Ag-SiO2The adhesive strength of soldering paste connection chip can steadily reach 27MPa or so.
(3) preparation process of the present invention is simple, high-efficient, and stability is good, at low cost.
Detailed description of the invention
Fig. 1: after the mixed proportion of embodiment 1, Ag-SiO2Nano-solder paste and nano mattisolda were tested in electrochemical migration
Leakage current in journey changes over time relational graph.Time when regulation leakage current value reaches 1mA is burn-out life, nano mattisolda
The average burn-out life be about 286min, Ag-SiO2The average burn-out life of nano-solder paste is 1029min, burn-out life phase
3.60 times are at least improved than nano mattisolda.
Specific embodiment
The present invention be by average particle size particle size be 20~100nm SiO 2 powder and diluent ultrasonic water bath association
Lower mixing is helped, object is mixed and is added in the nano mattisolda that average particle size particle size is 50~500nm, and mix by stirring
Uniformly obtained Ag-SiO2Nano-solder paste provides high efficiency preparation Ag-SiO under a kind of normal temperature condition2The method of nano-solder paste, system
The Ag-SiO obtained2Nano-solder paste function admirable, simple process and low cost, stability are good.Specific steps are as follows:
(a) it is equipped with the mixture of SiO 2 powder and diluent: the titanium dioxide for being 20~100nm by average particle size particle size
Si powder mixes 15~45min under the assistance of ultrasonic water bath with diluent (terpinol or ethyl alcohol)；
(b) it is equipped with the mixture of silver, SiO 2 powder and diluent: by the mixture of SiO 2 powder and diluent
It is added in the nano mattisolda that average particle size particle size is 50~500nm, obtains the mixing of silver, SiO 2 powder and diluent
Object；
(c) stir: the mixture of silver, SiO 2 powder and diluent that step (b) is obtained is 1000 by revolving speed
The high-efficiency stirring instrument of~2000r/min stirs 30~60s and Ag-SiO is made2Nano-solder paste.
Embodiment 1
(a) by average particle size particle size be 20~100nm SiO 2 powder and diluent terpinol in ultrasonic water bath
Lower mixing 30min is assisted, wherein the quality of SiO 2 powder is 0.1g, and the quality of terpinol is 0.1g；
(b) mixture of SiO 2 powder and diluent terpinol is added to average particle size particle size is 50~500nm
Nano mattisolda in, wherein the quality of silver paste be 113.52g, obtain silver, SiO 2 powder and terpinol mixture；
(c) mixture of the silver, SiO 2 powder and the terpinol that obtain step (b) is 2000r/min by revolving speed
High-efficiency stirring instrument stirring 60s be made Ag-SiO2Nano-solder paste.
Embodiment 2
(a) by average particle size particle size be 20~100nm SiO 2 powder and diluent terpinol in ultrasonic water bath
Lower mixing 15min is assisted, wherein the quality of SiO 2 powder is 5g, and the quality of terpinol is 7.5g；
(b) mixture of silicon dioxide powder and diluent terpinol is added to receiving for 50~500nm of average particle size particle size
In rice silver paste, wherein the quality of silver paste is 107.95g, obtains the mixture of silver, SiO 2 powder and terpinol；
(c) mixture of the silver, SiO 2 powder and the terpinol that obtain step (b) is 1500r/min by revolving speed
High-efficiency stirring instrument stirring 45s be made Ag-SiO2Nano-solder paste.
Embodiment 3
(a) by average particle size particle size be 20~100nm SiO 2 powder and diluent ethanol ultrasonic water bath association
Lower mixing 45min is helped, wherein the quality of SiO 2 powder is 15g, and the quality of ethyl alcohol is 30g；
(b) mixture of silicon dioxide powder and diluent ethanol is added to the nanometer of 50~500nm of average particle size particle size
In silver paste, wherein the quality of silver paste is 96.59g, obtains the mixture of silver, SiO 2 powder and ethyl alcohol；
(c) mixture of the silver, SiO 2 powder and the ethyl alcohol that obtain step (b) is 1000r/min's by revolving speed
High-efficiency stirring instrument stirs 30s and Ag-SiO is made2Nano-solder paste.
By Ag-SiO made from the embodiment of the present invention2Nano-solder paste and commercially-available nano mattisolda respectively with 5 DEG C/
The rate of heat addition of min is sintered at 280 DEG C, and furnace is cold after keeping the temperature 30min, then in 400 DEG C of hot conditions, 400V/mm electricity
Electromigration experiment is carried out under field intensity.As a result Ag-SiO is proved2The burn-out life of nano-solder paste compares the failure of nano mattisolda
Service life at least improves 3.60 times.
All methods that the present invention is disclosed and proposed, are described by preferred embodiment, related technical personnel
Can obviously the content of present invention not departed from, methods and techniques described herein route is being modified in spirit and scope or again
Combination, to realize final technology of preparing.Ag-SiO2Nano-solder paste can be obviously improved or inhibit when connecting high temperature power chip
The electromigration of silver, increases the burn-out life of electronic component, meets Electronic Packaging requirement.
Claims (8)
1. the Ag-SiO of resistance to silver electromigration under a kind of hot environment2The preparation method of nano-solder paste, it is characterized in that by average grain ruler
The very little SiO 2 powder for being 20~100nm mixes under the assistance of ultrasonic water bath with diluent；Then it is mixed object addition
In the nano mattisolda for being 50~500nm to average particle size particle size, and stir by mixing obtained Ag-SiO2Nanometer weldering
Cream.
2. the method as described in claim 1, it is characterized in that the Ag-SiO2The mass percent of silver paste in nano-solder paste
It is 99.82%~68.22%.
3. method according to claim 2, it is characterized in that the quality of the mixture of corresponding SiO 2 powder and diluent
Percentage is 0.18%~31.78%.
4. the method as described in claim 1, it is characterized in that the quality of the SiO 2 powder and the quality of diluent with
Than for 1:1~2.
5. the method as described in claim 1, it is characterized in that the diluent is alcohols solvent.
6. method as claimed in claim 5, it is characterized in that the diluent is terpinol or ethyl alcohol.
7. the method as described in claim 1, it is characterized in that mixing 15~45min under the assistance of ultrasonic water bath.
8. the method as described in claim 1, it is characterized in that being stirred in the case where revolving speed is the high-efficiency stirring instrument of 1000~2000r/min
Ag-SiO is made in 30~60s2Nano-solder paste.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811164526.8A CN109277723B (en) | 2018-10-06 | 2018-10-06 | Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811164526.8A CN109277723B (en) | 2018-10-06 | 2018-10-06 | Ag-SiO resistant to silver electromigration in high-temperature environment2Preparation method of nano soldering paste |
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| Publication Number | Publication Date |
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| CN109277723A true CN109277723A (en) | 2019-01-29 |
| CN109277723B CN109277723B (en) | 2021-08-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111230353A (en) * | 2020-01-19 | 2020-06-05 | 深圳第三代半导体研究院 | Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste |
| CN115026458A (en) * | 2022-06-17 | 2022-09-09 | 温州宏丰电工合金股份有限公司 | Ag-based alloy powder slurry, Ag-based alloy active solder and preparation method thereof |
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| JPH076623A (en) * | 1993-04-20 | 1995-01-10 | Ishizuka Glass Co Ltd | Conductive paste additive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111230353A (en) * | 2020-01-19 | 2020-06-05 | 深圳第三代半导体研究院 | Nano Ag-SnO for improving silver electromigration2Preparation method and application of solder paste |
| 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 |
| CN115026458A (en) * | 2022-06-17 | 2022-09-09 | 温州宏丰电工合金股份有限公司 | Ag-based alloy powder slurry, Ag-based alloy active solder and preparation method thereof |
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| CN109277723B (en) | 2021-08-03 |
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