CN107457502B - A kind of process preparing nano mattisolda based on Reverse Microemulsion System - Google Patents
A kind of process preparing nano mattisolda based on Reverse Microemulsion System Download PDFInfo
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- CN107457502B CN107457502B CN201710547706.3A CN201710547706A CN107457502B CN 107457502 B CN107457502 B CN 107457502B CN 201710547706 A CN201710547706 A CN 201710547706A CN 107457502 B CN107457502 B CN 107457502B
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- Prior art keywords
- reverse microemulsion
- microemulsion system
- aqueous solution
- nano mattisolda
- surfactant
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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
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention discloses a kind of processes that nano mattisolda is prepared based on Reverse Microemulsion System, include the following steps: the preparation of (1) mixed nitrate silver aqueous solution；(2) preparation of hydrazine hydrate solution；(3) it prepares polymer dielectric aqueous solution reverse micro emulsion, draw pseudoternary phase diagram；(4) preparation of nano mattisolda；(5) viscosity for adjusting the system soldering paste is interconnected to DBC substrate and IGBT power chip module.It is using technical solution of the present invention the utility model has the advantages that easy to operate, it can easily judge the formation of optimal reverse microemulsion system, solve the problems, such as that reverse microemulsion system stability is insufficient and nano particle is easy to happen reunion.
Description
Technical field
The present invention relates to the preparation technical fields of nano material, especially a kind of to prepare nanometer based on Reverse Microemulsion System
The process of silver paste.
Background technique
From after the promulgation of " made in China 2025 " development plan, industrial intelligent and greenization develop into theme, to intelligence
Can control chip and IGBT constant power semiconductor has greater demand.As that studies IGBT deepens continuously, find IGBT's
Various inefficacy mechanisms include summing up in the point that a little i.e. temperature factor in the failure modes such as overvoltage, overcurrent, excessively high junction temperature, di/dt
Influence.Theoretical and practice also indicates that, the operating temperature of device is every to increase 10 DEG C, and crash rate will increase l times or so, high-power
The Performance And Reliability of semiconductor devices and the temperature factor of device are closely connected.To adapt to severe working environment item
The continuous increase of part, power grade and power density is the irreversible developing direction of IGBT module, bears thermal stress to module
Requirement also further increase.
Using the IGBT module of welding encapsulating structure usually there are two welding layer, one is semiconductor chip and ceramic liner
Welding layer between plate, another is then the welding layer between ceramic lining plate and substrate.When IGBT module is in running order, core
Coefficient of thermal expansion mismatch makes welding layer bear cyclic stress in temperature changing process between piece, ceramic lining plate and substrate, most
Cause welding layer that thermal fatigue failure occurs eventually, reduces module long-term reliability.To reduce coefficient of thermal expansion mismatch between each layer
Influence, high pressure IGBT module selects AlN the and AlSiC material being more nearly with silicon thermal expansion coefficient as liner plate and base
Plate material.On the other hand, people also mention striving to find the method for improving welding layer quality and reducing welding layer voidage
Rise the reliability and heat dissipation performance of interconnection.
Novel high-quality chip-scale connecting material of the nano mattisolda as the alternative conventional solder of a new generation, conduction are led
The thermal efficiency is higher, and fusing point is high, and deelectric transferred ability is strong when work, is able to satisfy the growth requirement of present high performance components；Overcome
Conventional alloys solder high temperature reliability is not high and the glass transition temperature lower defect of conducting resinl.
105127435 A of Chinese invention patent specification CN discloses a kind of low temperature-sintered nano silver paste and preparation work
Skill, the patent of invention are described in detail the reverse microemulsion system constituted in the form of compound surfactant and carry out preparing nano silver
The method of slurry, but the method has the following shortcomings:
1, operating time and cumbersome especially judge whether to form optimal reverse microemulsion system inconvenient；
2, reverse microemulsion system stability is insufficient；
3, nano particle is easy to happen the problem of reunion.
Summary of the invention
Aiming at the shortcomings in the prior art, technical problem solved by the invention is can to operate during the preparation process letter
It is single, easily judge the formation of optimal reverse microemulsion system, solves reverse microemulsion system stability deficiency and nano particle holds
The problem of easily reuniting.
In order to solve the above technical problems, the technical solution adopted by the present invention is that a kind of received based on Reverse Microemulsion System preparation
The process of rice silver paste, includes the following steps:
(1) particles of silver nitrate is dissolved in distilled water and prepares certain density nitre by the preparation of mixed nitrate silver aqueous solution
Sour silver aqueous solution, is added dropwise the polymer dielectric of different quality, prepares the mixing containing different polymer electrolyte amount percentages
Silver nitrate aqueous solution；
(2) hydrazine hydrate solution is dissolved in distilled water and obtains certain density hydrazine hydrate solution by the preparation of hydrazine hydrate solution；
(3) it prepares polymer dielectric aqueous solution reverse micro emulsion, draw pseudoternary phase diagram；
If surfactant, cosurfactant are respectively m1, m2, m3 with oily phase organic matter quality, different m1/m2 are taken
Value first assumes that (m1+m2): m3=1:1 is optimal proportion, and surfactant, cosurfactant and oily phase organic matter are successively added
It is added in beaker, the mixed nitrate silver containing different polymer electrolyte amount percentages is added dropwise while stirring at a constant temperature
Aqueous solution, the volume of mixed nitrate silver aqueous solution and determining optimal m1/ when record system changes in " muddiness-clarification-muddiness "
M2 value；
Fixed m1/m2 value, takes difference (m1+m2)/m3, by surfactant, cosurfactant and oil phase organic matter according to
It is secondary to be added in beaker, at a constant temperature, mixed nitrate silver aqueous solution is added dropwise while stirring, record system is in " muddy-clear
The volume of mixed nitrate silver aqueous solution when clearly-muddiness " variation；
The modified reverse microemulsion system of best polymer electrolyte is determined simultaneously according to the amount of solubilized maximum mixed nitrate silver
Draw pseudoternary phase diagram；
(4) preparation of nano mattisolda determines optimal Reverse Microemulsion System according to pseudoternary phase diagram, into system by
Hydrazine hydrate solution is added dropwise in drop, obtains the reverse micro emulsion containing nano-Ag particles, then be centrifuged to obtain and be adsorbed by organic matter
Nano-Ag particles；
(5) viscosity for adjusting the system soldering paste is interconnected to DBC substrate and IGBT power chip module.
The surfactant constituent is nonionic surfactant or Gemini(Shuangzi) surfactant.
The cosurfactant uses carbon atom number for the alcohol of 3-6.
The oil phase organic matter uses carbon atom number for the alkane of 5-8.
The polymer dielectric uses the cationic polymer electrolyte with high charge density.
Using technical solution of the present invention the utility model has the advantages that
1, operating procedure and the time of half, faster easier judgement are saved in the operation for exploring Optimal system
Whether optimal reverse microemulsion system is formed.
2, the stability and reverse phase of Interaction enhanced between polymer dielectric and surfactant droplet interfaces are micro-
The stability of newborn system solves the problems, such as that reverse microemulsion system stability is insufficient.
3, make individually to be lived by surface there are the electrostatic reprimand effect between polymer dielectric and non-ionic surface active in soldering paste
Property agent package nano-Ag particles be not easy to be merged into one piece, than individually being prevented with the nano-Ag particles of surfactant package
Agglomeration traits have better effect, and solve the problems, such as that nano particle is easy to happen reunion.
Detailed description of the invention
Fig. 1 is flow chart of the invention.
Specific embodiment
A specific embodiment of the invention is further described with reference to the accompanying drawings and examples, but is not to this hair
Bright restriction.
Fig. 1 shows process of the invention, a kind of process preparing nano mattisolda based on Reverse Microemulsion System,
Include the following steps:
(1) particles of silver nitrate is dissolved in distilled water and prepares certain density nitre by the preparation of mixed nitrate silver aqueous solution
Sour silver aqueous solution, is added dropwise the polymer dielectric of different quality, prepares the mixing containing different polymer electrolyte amount percentages
Silver nitrate aqueous solution；
(2) hydrazine hydrate solution is dissolved in distilled water and obtains certain density hydrazine hydrate solution by the preparation of hydrazine hydrate solution；
(3) it prepares polymer dielectric aqueous solution reverse micro emulsion, draw pseudoternary phase diagram；
If surfactant, cosurfactant are respectively m1, m2, m3 with oily phase organic matter quality, different m1/m2 are taken
Value first assumes that (m1+m2): m3=1:1 is optimal proportion, and surfactant, cosurfactant and oily phase organic matter are successively added
It is added in beaker, the mixed nitrate silver containing different polymer electrolyte amount percentages is added dropwise while stirring at a constant temperature
Aqueous solution, the volume of mixed nitrate silver aqueous solution and determining optimal m1/ when record system changes in " muddiness-clarification-muddiness "
M2 value；
Fixed m1/m2 value, takes difference (m1+m2)/m3, by surfactant, cosurfactant and oil phase organic matter according to
It is secondary to be added in beaker, at a constant temperature, mixed nitrate silver aqueous solution is added dropwise while stirring, record system is in " muddy-clear
The volume of mixed nitrate silver aqueous solution when clearly-muddiness " variation；
The modified reverse microemulsion system of best polymer electrolyte is determined simultaneously according to the amount of solubilized maximum mixed nitrate silver
Draw pseudoternary phase diagram；
(4) preparation of nano mattisolda determines optimal Reverse Microemulsion System according to pseudoternary phase diagram, into system by
Hydrazine hydrate solution is added dropwise in drop, obtains the reverse micro emulsion containing nano-Ag particles, then be centrifuged to obtain and be adsorbed by organic matter
Nano-Ag particles；
(5) viscosity for adjusting the system soldering paste is interconnected to DBC substrate and IGBT power chip module.
The surfactant is nonionic surfactant；
The surfactant is Gemini(Shuangzi) surfactant；
This example surfactant is one in Triton X-100, PVP, 12-3-12 type Gemini(Shuangzi) quaternary ammonium salt
Kind.
The cosurfactant uses carbon atom number for the alcohol of 3-6, and this example is one of n-hexyl alcohol, isopropanol.
The oil phase organic matter uses carbon atom number for the alkane of 5-8, and this example is one of normal heptane, hexamethylene.
The polymer dielectric uses the cationic polymer electrolyte with high charge density, and this example is polyethyleneimine
Amine.
Embodiment 1
A kind of preparation process of nano mattisolda, includes the following steps:
1) preparation of mixed nitrate silver aqueous solution: it is 0.1mol/L that particles of silver nitrate, which is dissolved in distilled water, and prepares concentration
Silver nitrate aqueous solution, and to the polyethyleneimine (PEI) of silver nitrate aqueous solution dropwise addition different quality, prepare matter containing polyethyleneimine
Amount percentage is respectively 0.1%, 0.5%, 1%, 5%, 10% mixed nitrate silver aqueous solution；
2) preparation of hydrazine hydrate solution: hydrazine hydrate solution is dissolved in obtained in distilled water 0.5mol/L hydrazine hydrate it is molten
Liquid；
3) it prepares polymer dielectric aqueous solution reverse micro emulsion, draw pseudoternary phase diagram:
Note Triton X-100, n-hexyl alcohol and normal heptane quality are respectively m1, m2, m3, take m1:m2=(9:1,8:2,7:3,
6:4,5:5,4:6,3:7,2:8,1:9), (m1+m2): m3=1:1 successively adds Triton X-100, n-hexyl alcohol and normal heptane
Into beaker, mixed nitrate silver aqueous solution is added dropwise while stirring at a constant temperature, record system is in " muddiness-clarification-is muddy
It is turbid " variation when mixed nitrate silver aqueous solution volume and determine m1/m2 value.
Fixed m1/m2 value, takes difference (m1+m2): m3=(9:1,8:2,7:3,6:4,5:5,4:6,3:7,2:8,1:9), will
Surfactant, cosurfactant and oily phase organic matter are successively added in beaker, under 30 DEG C of steady temperatures while stirring
The mixed nitrate silver aqueous solution that mass percent containing polyethyleneimine is respectively 0.1%, 0.5%, 1%, 5%, 10% is added dropwise, records body
The volume of mixed nitrate silver aqueous solution when system changes in " muddiness-clarification-muddiness ".
To determine optimal reverse microemulsion system and pseudoternary phase diagram is drawn according to the amount of solubilized maximum mixed nitrate silver.
4) preparation of nano mattisolda: determining optimal Reverse Microemulsion System according to the pseudoternary phase diagram of step 3, then to
The hydrazine hydrate solution of 0.5mol/L is added dropwise in system dropwise, can react to obtain the reverse micro emulsion containing nano-Ag particles；Then
It is centrifuged to obtain the nano-Ag particles adsorbed by organic matter.
5) viscosity for adjusting the system soldering paste is interconnected to DBC substrate and IGBT power chip module.
Embodiment 2
According to the identical method of embodiment 1, use PVP substitution Triton X-100 for surfactant, and with n-hexyl alcohol
For cosurfactant, normal heptane is oily phase organic matter, and polyethyleneimine is modified anti-for stabilizer composition polymer dielectric
Phase microemulsion system prepares nano mattisolda.
Embodiment 3
According to the identical method of embodiment 1, using 12-3-12 type Gemini(Shuangzi) quaternary ammonium salt substitution Triton X-
100 be surfactant, and using n-hexyl alcohol as cosurfactant, and normal heptane is oily phase organic matter, and polyethyleneimine is to stablize
Agent constitutes the modified Reverse Microemulsion System of polymer dielectric and prepares nano mattisolda.
Embodiment 4
According to the identical method of embodiment 1, use isopropanol substitution n-hexyl alcohol for cosurfactant, and with Triton
X-100 is surfactant, and normal heptane is oily phase organic matter, and polyethyleneimine is that stabilizer constitutes what polymer dielectric was modified
Reverse Microemulsion System prepares nano mattisolda.
Embodiment 5
According to the identical method of embodiment 1, use isopropanol substitution n-hexyl alcohol for cosurfactant, and using PVP as table
Face activating agent, normal heptane are oily phase organic matter, and polyethyleneimine is that stabilizer constitutes the modified reverse microemulsion of polymer dielectric
Liquid system prepares nano mattisolda.
Embodiment 6
According to the identical method of embodiment 1, use hexamethylene substitution normal heptane for oily phase organic matter, Triton X-100 is
Surfactant, n-hexyl alcohol are cosurfactant, and polyethyleneimine is that stabilizer constitutes the modified reverse phase of polymer dielectric
Microemulsion system prepares nano mattisolda.
Detailed description is made that embodiments of the present invention in conjunction with attached drawing above, but the present invention be not limited to it is described
Embodiment.To those skilled in the art, without departing from the principles and spirit of the present invention, to these implementations
Mode carries out various change, modification, replacement and variant are still fallen in protection scope of the present invention.
Claims (10)
1. a kind of process for preparing nano mattisolda based on Reverse Microemulsion System, characterized by the following steps:
(1) particles of silver nitrate is dissolved in distilled water and prepares certain density silver nitrate by the preparation of mixed nitrate silver aqueous solution
The polymer dielectric of different quality is added dropwise in aqueous solution, prepares the mixed nitrate containing different polymer electrolyte amount percentages
Silver-colored aqueous solution；
(2) hydrazine hydrate solution is dissolved in distilled water and obtains certain density hydrazine hydrate solution by the preparation of hydrazine hydrate solution；
(3) it prepares polymer dielectric aqueous solution reverse micro emulsion, draw pseudoternary phase diagram；
If surfactant, cosurfactant are respectively m1, m2, m3 with oily phase organic matter quality, different m1/m2 values are taken, first
Assuming that (m1+m2): m3=1:1 is optimal proportion, and surfactant, cosurfactant and oily phase organic matter are successively added to
In beaker, it is water-soluble that the mixed nitrate silver containing different polymer electrolyte amount percentages is added dropwise while stirring at a constant temperature
Liquid, the volume of mixed nitrate silver aqueous solution and determining optimal m1/m2 value when record system changes in " muddiness-clarification-muddiness "；
Fixed m1/m2 value, takes difference (m1+m2)/m3, and surfactant, cosurfactant and oily phase organic matter are successively added
It is added in beaker, at a constant temperature, mixed nitrate silver aqueous solution is added dropwise while stirring, record system is in " muddiness-clarification-
The volume of mixed nitrate silver aqueous solution when muddiness " variation；
The modified reverse microemulsion system of best polymer electrolyte is determined according to the amount of solubilized maximum mixed nitrate silver and is drawn
Pseudoternary phase diagram；
(4) preparation of nano mattisolda determines optimal Reverse Microemulsion System according to pseudoternary phase diagram, drips dropwise into system
Add hydrazine hydrate solution, obtain the reverse micro emulsion containing nano-Ag particles, then is centrifuged to obtain receiving by organic matter absorption
Rice Argent grain；
(5) viscosity for adjusting the system soldering paste is interconnected to DBC substrate and IGBT power chip module.
2. the process according to claim 1 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the surfactant is nonionic surfactant.
3. the process according to claim 1 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the surfactant is Gemini Gemini surface active agent.
4. the process according to claim 2 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the surfactant is PVP or Triton X-100.
5. the process according to claim 1 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the cosurfactant uses carbon atom number for the alcohol of 3-6.
6. the process according to claim 5 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the cosurfactant is n-hexyl alcohol or isopropanol.
7. the process according to claim 1 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the oil phase organic matter uses carbon atom number for the alkane of 5-8.
8. the process according to claim 7 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the oil phase organic matter is normal heptane or hexamethylene.
9. the process according to claim 1 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the polymer dielectric uses the cationic polymer electrolyte with high charge density.
10. the process according to claim 9 for being prepared nano mattisolda based on Reverse Microemulsion System, feature are existed
In: the polymer dielectric is polyethyleneimine.
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| CN1437200A (en) * | 2003-01-14 | 2003-08-20 | 中山大学 | Low-content nanometer conducting silver paste and its prepn |
| CN101381423A (en) * | 2008-09-10 | 2009-03-11 | 厦门大学 | Method for preparing silver-coating polystyrene nano granule |
| CN102248175A (en) * | 2011-05-30 | 2011-11-23 | 东华大学 | Method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion |
| KR101239262B1 (en) * | 2011-04-27 | 2013-03-06 | 고려대학교 산학협력단 | method for manufacturing silica-ceria, core-shell nanoparticles using microemulsion |
| CN105127439A (en) * | 2014-05-27 | 2015-12-09 | 北京化工大学 | Preparation method for oil-phase silver nanoparticles |
| CN105127435A (en) * | 2015-09-24 | 2015-12-09 | 桂林电子科技大学 | Low-temperature sintering nano-silver paste and preparation process thereof |
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2017
- 2017-07-06 CN CN201710547706.3A patent/CN107457502B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1437200A (en) * | 2003-01-14 | 2003-08-20 | 中山大学 | Low-content nanometer conducting silver paste and its prepn |
| CN101381423A (en) * | 2008-09-10 | 2009-03-11 | 厦门大学 | Method for preparing silver-coating polystyrene nano granule |
| KR101239262B1 (en) * | 2011-04-27 | 2013-03-06 | 고려대학교 산학협력단 | method for manufacturing silica-ceria, core-shell nanoparticles using microemulsion |
| CN102248175A (en) * | 2011-05-30 | 2011-11-23 | 东华大学 | Method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion |
| CN105127439A (en) * | 2014-05-27 | 2015-12-09 | 北京化工大学 | Preparation method for oil-phase silver nanoparticles |
| CN105127435A (en) * | 2015-09-24 | 2015-12-09 | 桂林电子科技大学 | Low-temperature sintering nano-silver paste and preparation process thereof |
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