CN110102934A - A kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material - Google Patents
A kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material Download PDFInfo
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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
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Abstract
The present invention relates to a kind of preparation methods of electrochemically resistant migration-type nano silver composite solder paste material, belong to technical field of welding materials.Technical solution of the present invention uses the compound scheme of colloidal sol, palladium nickel complex sol and silver nano-grain progress is effectively compound, due to passing through sol-gal process, the Pd atom dispersion on duplex metal nano granule surface is more uniform, simultaneously, since nano silver is easy to reunite, in order to prevent the reunion of nano silver, using surfactant, micella is formed on silver particles surface in a manner of lying low, as one layer of steric hindrance layer, the reunion of nano silver is prevented to grow up, simultaneously because complex sol material face is negatively charged, and the surfactant of Argent grain adsorption keeps nanometer silver surface positively charged, deposition of the surfactant to composite gel particle in nanometer silver surface plays orientation, ultimately form the composite particles of core-shell structure, keep it not easy to reunite and disperses, further improve the structural strength and dispersion performance of material.
Description
Technical field
The present invention relates to a kind of preparation methods of electrochemically resistant migration-type nano silver composite solder paste material, belong to welding material
Technical field.
Background technique
The research that metallic silver is used as encapsulation connecting material can be traced back into last century the eighties, by micron-sized silver
Grain and silver strip are as connecting material, and the pressure for applying about 40MPa realizes chip and substrate in low temperature as sintering driving force
Under connection.The sintering mechanism of above-mentioned law temperature joining technology is solid-state diffusion and the densification process caused, due to sintering process
It is middle to need to be consequently belonging to pressure assisted sintering as sintering driving force by external pressure.Test proves, assists burning using pressure
Knot technology, sintering temperature is minimum to be down to 250 DEG C, and the consistency of chip and substrate articulamentum can reach 85%, and jointing
With good electrical, thermal and mechanical properties, bonding strength is up to stable 30MPa.However, this pressure assisted sintering technology
Additional process equipment is needed, it is at high cost and complicated for operation, and apply excessively high pressure and will cause the failure of chip and substrate.
Therefore, it should take measures suitably to reduce the pressure of required application when even removal sintering.Many researchers are by reducing Argent grain
Size to submicron order and apply the sintering driving force of the pressure of several megapascal as auxiliary, realize between chip and substrate
Connection.To the beginning of this century, the particle size of Argent grain is reduced to Nano grade, and add organic principle to improve its viscosity, system
At nano mattisolda.The silver powder and sheet silver that it replaces micron level successfully reduce sintering as novel connecting material
Temperature and necessary aux. pressure, it might even be possible under conditions of no pressure, realize between power semiconductor and substrate
Connection.The sintering mechanism of nano mattisolda is similar to the sintering mechanism of the silver powder of micron level and sheet silver, is all by solid
Mutually the densification of silver-colored articulamentum is realized in diffusion.Unlike, the sintering process of sheet silver needs to apply ambient pressure as sintering
Driving force, and for nano mattisolda, the silver particles of Nano grade surface energy with higher provides driving for sintering
Power, it is no longer necessary to apply pressure assisted sintering.However, things always has dual character, although the silver particles of Nano grade are that sintering mentions
Driving force is supplied, but it is reunited and intergranular polymerism is very serious.In order to solve this problem, pass through
Surfactant (usually fatty acid group), diluent (the usually polymer of low molecular weight) etc. are added to prevent between particle
Reunion and polymerization phenomena such as generation.
About being the discovery that for the first time in the lab for silver-colored electrochemical migration phenomenon, on the silver-plated terminal of telephone exchange
It was found that, they think that the phenomenon is as caused by higher voltage and higher ambient humidity.In addition, research worker is also right
Common metal has carried out electrochemical migration test in power semiconductor package, the results showed that, electrochemical migration occurs for metal
Sensibility is by by force to weak sequence are as follows: Ag, Pb, Cu, Zn.Therefore, silver is one of the metal for being easiest to occur electrochemical migration.To mesh
Before until, many scholars expand a large amount of research for the electrochemical migration phenomenon of silver, such as the influence of silver-colored electrochemical migration
Factor, silver electricity migration mechanism (room temperature wet environment and high temperature drying environment) and improve the electrochemical migration behavior of silver
Measure etc..Research shows that DC voltage between electrode, electrode spacing, environment temperature and dielectric substrate material etc. are all to influence silver electricity
The possible factor of chemical transport.
All the time, Sn-Pb solder is widely used in the advantages that its good wetability, soldering reliability and stability
In electronics industry.However, Pb is containing toxic, pollution environment and the life quality for seriously affecting the mankind and livestock.It is protected based on environment
The requirement of shield, the unleaded of electronic product have also been put on schedule.As European Union passes through electronic electric equipment instruction and electronics electricity
The instruction of certain harmful substances is forbidden to use in gas equipment, China is directed to the arrival of unleaded trend, has also put into effect " electronic information
Estate Division pollutes protection management method ".Electronics industry appeals that, using environment-friendly electronic material, electronic product has to unleaded turn
Become, the research and development of unleaded solder is extremely urgent.Using Sn as matrix, the solder of the metals such as Ag, Cu, Sb, In is added
Alloy is lead-free solder most commonly used in current power semiconductor device package.SnAgCu and SnCu two class solder among these
Using being widest.The eutectic temperature of SnAgCu solder is higher than SnPb solder, and high-temperature stability is good, and the gold that eutectic is formed
Compound disperses are distributed on matrix between category, good mechanical performance；The disadvantage is that wetability is poor with respect to SnPb solder.SnCu solder
The advantages of be that cost of material is cheap；The disadvantage is that wetability is poor, poor mechanical property.Therefore, it is compared with SnPb solder, lead-free solder is still
The main problems such as poor, fusing point height that there are wetabilitys.
Nano mattisolda for power semiconductor device package is with its high-melting-point, excellent electricity, hot property and green
The advantages that unleaded, gradually replaces traditional tin-lead solder and leadless welding alloy as novel chip-scale interconnection material.However
A large number of studies show that silver is a kind of metal easily migrated, silver-colored electrochemical migration can change dielectric properties, reduce exhausted
Edge resistance leads to the generation of short circuit and promotes equipment failure.The electrochemical migration of silver, which proposes the reliability of power package, to be chosen
War, many scholars also proposed corresponding Improving Measurements, but all be directed to room temperature wet environment.Existing research at present has found that silver exists
Electrochemical migration phenomenon under high temperature drying environment.The development applied in high temperature with wide bandgap semiconductor, nano mattisolda
As chip connecting material, a possibility that electrochemical migration occurs, will be greatly increased, this will become electronic component and for a long time may be used
By the secret worry of work.But directly prepare that the composite solder paste material of compound Ag and Pb its mechanical property is poor, and bond strength is not high,
Its service life is caused to be greatly reduced, so being effectively modified to it necessary.
Summary of the invention
The technical problems to be solved by the invention: for traditional composite solder paste material for directly preparing compound Ag and Pb its
The problem of mechanical property is poor, and bond strength is not high, its service life is caused to be greatly reduced provides a kind of electrochemically resistant migration
The preparation method of type nano silver composite solder paste material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of 8% poly-vinyl alcohol solutions of mass fraction,
10~15 parts of palladium chloride solutions, 15~20 parts of nickel chloride solutions are placed in conical flask, are led to nitrogen and are excluded air again in nitrogen gas
Insulated and stirred under atmosphere obtains reaction solution and in mass ratio 1:25, and 2% boron hydracid sodium solution of mass fraction is added dropwise in reaction solution,
It is stood after insulation reaction, obtains complex sol liquid；
(2) according to parts by weight, it is molten that 45~50 parts of deionized waters, the sour sodium of 10~15 parts of 10% lemons of mass fraction three are weighed respectively
Liquid, 3~5 parts of 1% nitric acid of mass fraction and 1~2 part of 1% boron hydracid sodium solution of mass fraction are placed in blender, are stirred
And 25~30s is stood, obtain seed liquor；
(3) again according to parts by weight, 45~50 parts of deionized waters, 1~2 part of cetyl trimethylammonium bromide and 1 are weighed respectively
~2 parts of 0.1mol/L ascorbic acid solutions are placed in a beaker, and are stirred and adjust pH to 7.0, are stirred to obtain matrix reaction
Seed liquor is added dropwise in matrix reaction solution by liquid in 1:5 in mass ratio, is stirred and ultrasonic disperse, must disperse slurries and by
Mass ratio 1:2, will dispersion slurries and complex sol liquid to be stirred juxtaposition still aging at room temperature, collect to obtain compound ageing liquid
And rotary evaporation is handled, and collects dry colloidal sol；
(4) dry colloidal sol is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, after the completion of being passed through, heating heating, heat preservation is forged
Calcining materials are burnt and collect, standing is cooled to room temperature and is ground up, sieved, and obtains modified composite Nano Argent grain；According to parts by weight,
It is molten that 45~50 parts of neopelexes, 45~50 parts of deionized waters, 3~5 parts of 5% polyvinyl alcohol of mass fraction are weighed respectively
Liquid and 6~8 parts of composite Nano Argent grains are placed in blender, are stirred and are adjusted using dilution dilution agent, can be prepared into
The electrochemically resistant migration-type nano silver composite solder paste material.
It is 25~30mL/min that the nitrogen, which is passed through rate,.
The insulated and stirred temperature is 0~5 DEG C.
It is 1.0~1.5mL/min that drop rate, which is added dropwise, in the 2% boron hydracid sodium solution of amount score.
The rotary evaporation processing is rotary evaporated to dryness at 45~50 DEG C.
The nickel chloride solution is 1:15 in mass ratio, and nickel chloride is added in deionized water, chlorine is stirred to obtain
Change nickel solution.
The palladium chloride solution is 1:15 in mass ratio, and palladium chloride is added in deionized water, chlorine is stirred to obtain
Change palladium solution.
The diluent is preferably terpinol.
The dilution is adjusted to be adjusted to solid content with diluent to be 70%.The present invention is compared with other methods, beneficial
It has the technical effect that
(1) technical solution of the present invention uses the compound scheme of colloidal sol, and palladium nickel complex sol and silver nano-grain progress is effectively compound,
Since by sol-gal process, the Pd atom dispersion on duplex metal nano granule surface is more uniform, while Pd/Ni bimetal nano
In particle, simultaneously electric charge transfer occurs for Pd atom and Ni atomic interaction so that Pd atom is negatively charged and Ni atom is positively charged, make
There is integral material excellent electronically active, in order to prevent the reunion of nano silver, to adopt simultaneously as nano silver is easy to reunite
With surfactant, mainly its there are two effects: first, due to the effect of charge, surfactant in a manner of lying low
Silver particles surface forms micella as one layer of steric hindrance layer and the reunion of nano silver is prevented to grow up；Second, due to complex sol material
Face is negatively charged, and the surfactant of Argent grain adsorption keeps nanometer silver surface positively charged, attracts each other in positive and negative charge
Under the action of, deposition of the surfactant to composite gel particle in nanometer silver surface plays orientation, ultimately forms nucleocapsid
The composite particles of structure, the composite material being prepared have excellent structural behaviour, keep it not easy to reunite and disperse, further
Improve the structural strength and dispersion performance of material；
(2) in the technical solution of the present invention, technical solution of the present invention is modified using the composite material of Pd/Ag, due to from material
Material thermodynamics set out, and the effect of the alloying of composite particles can be explained by ideal solution approximate model, from macroscopic angle
Degree, if A, B mix the atom of two kinds of constituent elements or molecule, both without generating fuel factor or without generating bulk effect,
Be formed by solution then as ideal solution, that is, formed idea solid solution macroscopic conditions be two constituent elements answer structure having the same and
Lattice constant, microcosmic requirement be constitute solution two constituent elements atom bond energy before mixing should with mix after generated new keys
Bond energy it is identical, i.e., mixing in be able to maintain it is constant, since silver-colored simple substance and palladium simple substance can form continuous solid solution, lattice constant phase
Closely, the atomic property of the two is close, and crystal structure is identical, i.e. " similar to mix ", when two kinds of atoms are mixed, compared to tradition
Nano mattisolda, nano combined soldering paste can form continuous solid solution alloy at high temperature, so that the free energy of system drops to
Minimum, to enhance its thermodynamic stability, sintering silver is then not susceptible to oxidation, decomposes, and has delayed the electricity of compound ion
From, transition process, electrochemical migration burn-out life value is also increased accordingly.
Specific embodiment
Palladium chloride is added in deionized water by 1:15 in mass ratio, is stirred to obtain palladium chloride solution, then in mass ratio
Nickel chloride is added in deionized water by 1:15, is stirred to obtain nickel chloride solution, then according to parts by weight, weighs 45 respectively
~50 parts of deionized waters, 10~15 parts of 8% poly-vinyl alcohol solutions of mass fraction, 10~15 parts of palladium chloride solutions, 15~20 parts of chlorine
Change nickel solution to be placed in conical flask, it is 25~30mL/min that control nitrogen, which is passed through rate, leads to nitrogen and excludes air again in nitrogen
It is placed in 25~30min of insulated and stirred at 0~5 DEG C under atmosphere, obtains reaction solution and in mass ratio 1:25, by 2% boron hydrogen of mass fraction
Acid sodium solution is added dropwise in reaction solution, and control drop rate is 1.0~1.5mL/min, after 1~2h of insulation reaction, stand 3~
5h obtains complex sol liquid；According to parts by weight, 45~50 parts of deionized waters, 10~15 parts of 10% lemons of mass fraction are weighed respectively
Three acid sodium solution of lemon, 3~5 parts of 1% nitric acid of mass fraction and 1~2 part of 1% boron hydracid sodium solution of mass fraction are placed in blender
In, it is stirred and is stood 25~30s, obtains seed liquor；Again according to parts by weight, respectively weigh 45~50 parts of deionized waters, 1~
2 parts of cetyl trimethylammonium bromides and 1~2 part of 0.1mol/L ascorbic acid solution are placed in a beaker, and are stirred and are adjusted
PH to 7.0 is stirred to obtain matrix reaction solution, and in 1:5 in mass ratio, seed liquor is added dropwise in matrix reaction solution, and stirring is mixed
Merge collect be placed in 10~15min of ultrasonic disperse under 200~300W, must disperse slurries and 1:2 in mass ratio, will disperse slurries and
Complex sol liquid is stirred juxtaposition still aging 3~5h at room temperature, collect compound ageing liquid is placed at 45~50 DEG C
Rotary evaporated to dryness is collected dry colloidal sol and is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, control nitrogen is passed through rate and is
25~30mL/min is warming up to 850~900 DEG C after the completion of being passed through, then by 5 DEG C/min, and calcining materials are calcined and collected in heat preservation,
Standing is cooled to room temperature and ground 200 mesh, obtains modified composite Nano Argent grain；According to parts by weight, 45~50 are weighed respectively
Part neopelex, 45~50 parts of deionized waters, 3~5 parts of 5% poly-vinyl alcohol solutions of mass fraction and 6~8 parts are compound
Nano-Ag particles are placed in blender, are stirred and diluent is used to be adjusted to solid content as 70%, can be prepared into described
Electrochemically resistant migration-type nano silver composite solder paste material.The diluent is preferably terpinol.
Palladium chloride is added in deionized water by 1:15 in mass ratio, is stirred to obtain palladium chloride solution, then in mass ratio
Nickel chloride is added in deionized water by 1:15, is stirred to obtain nickel chloride solution, then according to parts by weight, weighs 45 respectively
Part deionized water, 10 parts of 8% poly-vinyl alcohol solutions of mass fraction, 10 parts of palladium chloride solutions, 15 parts of nickel chloride solutions are placed in triangle
In flask, it is 25mL/min that control nitrogen, which is passed through rate, and logical nitrogen exclusion air is placed in heat preservation at 0 DEG C in a nitrogen atmosphere again and stirs
25min is mixed, reaction solution and in mass ratio 1:25 are obtained, 2% boron hydracid sodium solution of mass fraction is added dropwise in reaction solution, control drop
Rate of acceleration is 1.0mL/min, after insulation reaction 1h, stands 3h, obtains complex sol liquid；According to parts by weight, 45 parts are weighed respectively
Deionized water, 10 parts of 10% lemon of mass fraction, three acid sodium solutions, 3 parts of 1% nitric acid of mass fraction and 1 part of 1% boron of mass fraction
Hydracid sodium solution is placed in blender, is stirred and is stood 25s, obtain seed liquor；Again according to parts by weight, 45 parts are weighed respectively
Deionized water, 1 part of cetyl trimethylammonium bromide and 1 part of 0.1mol/L ascorbic acid solution are placed in a beaker, and are stirred
And pH to 7.0 is adjusted, it is stirred to obtain matrix reaction solution, in 1:5 in mass ratio, seed liquor is added dropwise in matrix reaction solution,
It is stirred and collects and be placed in ultrasonic disperse 10min under 200W, slurries and 1:2 in mass ratio must be dispersed, by dispersion slurries and again
Close sol solutions be stirred juxtaposition still aging 3h at room temperature, collect compound ageing liquid be placed at 45 DEG C rotate be evaporated to
It is dry, it collects dry colloidal sol and is placed in tube-type atmosphere furnace, lead to nitrogen and exclude air, it is 25mL/min that control nitrogen, which is passed through rate,
850 DEG C are warming up to after the completion of being passed through, then by 5 DEG C/min, calcining materials are calcined and collected in heat preservation, and standing is cooled to room temperature and grinds
Honed 200 mesh obtains modified composite Nano Argent grain；According to parts by weight, 45 parts of neopelexes, 45 parts are weighed respectively
Deionized water, 3 parts of 5% poly-vinyl alcohol solutions of mass fraction and 6 parts of composite Nano Argent grains are placed in blender, are stirred simultaneously
It uses diluent to be adjusted to solid content as 70%, the electrochemically resistant migration-type nano silver composite solder paste material can be prepared into
Material.The diluent is preferably terpinol.
Palladium chloride is added in deionized water by 1:15 in mass ratio, is stirred to obtain palladium chloride solution, then in mass ratio
Nickel chloride is added in deionized water by 1:15, is stirred to obtain nickel chloride solution, then according to parts by weight, weighs 47 respectively
Part deionized water, 12 parts of 8% poly-vinyl alcohol solutions of mass fraction, 12 parts of palladium chloride solutions, 17 parts of nickel chloride solutions are placed in triangle
In flask, it is 27mL/min that control nitrogen, which is passed through rate, and logical nitrogen exclusion air is placed in heat preservation at 2 DEG C in a nitrogen atmosphere again and stirs
27min is mixed, reaction solution and in mass ratio 1:25 are obtained, 2% boron hydracid sodium solution of mass fraction is added dropwise in reaction solution, control drop
Rate of acceleration is 1.2mL/min, after insulation reaction 2h, stands 4h, obtains complex sol liquid；According to parts by weight, 47 parts are weighed respectively
Deionized water, 12 parts of 10% lemon of mass fraction, three acid sodium solutions, 4 parts of 1% nitric acid of mass fraction and 2 parts of 1% boron of mass fraction
Hydracid sodium solution is placed in blender, is stirred and is stood 27s, obtain seed liquor；Again according to parts by weight, 44 parts are weighed respectively
Deionized water, 1 part of cetyl trimethylammonium bromide and 12 parts of 0.1mol/L ascorbic acid solutions are placed in a beaker, and are stirred
And pH to 7.0 is adjusted, it is stirred to obtain matrix reaction solution, in 1:5 in mass ratio, seed liquor is added dropwise in matrix reaction solution,
It is stirred and collects and be placed in ultrasonic disperse 12min under 250W, slurries and 1:2 in mass ratio must be dispersed, by dispersion slurries and again
Close sol solutions be stirred juxtaposition still aging 4h at room temperature, collect compound ageing liquid be placed at 47 DEG C rotate be evaporated to
It is dry, it collects dry colloidal sol and is placed in tube-type atmosphere furnace, lead to nitrogen and exclude air, it is 27mL/min that control nitrogen, which is passed through rate,
875 DEG C are warming up to after the completion of being passed through, then by 5 DEG C/min, calcining materials are calcined and collected in heat preservation, and standing is cooled to room temperature and grinds
Honed 200 mesh obtains modified composite Nano Argent grain；According to parts by weight, 47 parts of neopelexes, 47 parts are weighed respectively
Deionized water, 4 parts of 5% poly-vinyl alcohol solutions of mass fraction and 7 parts of composite Nano Argent grains are placed in blender, are stirred simultaneously
It uses diluent to be adjusted to solid content as 70%, the electrochemically resistant migration-type nano silver composite solder paste material can be prepared into
Material.The diluent is preferably terpinol.
Palladium chloride is added in deionized water by 1:15 in mass ratio, is stirred to obtain palladium chloride solution, then in mass ratio
Nickel chloride is added in deionized water by 1:15, is stirred to obtain nickel chloride solution, then according to parts by weight, weighs 50 respectively
Part deionized water, 15 parts of 8% poly-vinyl alcohol solutions of mass fraction, 15 parts of palladium chloride solutions, 20 parts of nickel chloride solutions are placed in triangle
In flask, it is 30mL/min that control nitrogen, which is passed through rate, and logical nitrogen exclusion air is placed in heat preservation at 5 DEG C in a nitrogen atmosphere again and stirs
30min is mixed, reaction solution and in mass ratio 1:25 are obtained, 2% boron hydracid sodium solution of mass fraction is added dropwise in reaction solution, control drop
Rate of acceleration is 1.5mL/min, after insulation reaction 2h, stands 5h, obtains complex sol liquid；According to parts by weight, 50 parts are weighed respectively
Deionized water, 15 parts of 10% lemon of mass fraction, three acid sodium solutions, 5 parts of 1% nitric acid of mass fraction and 2 parts of 1% boron of mass fraction
Hydracid sodium solution is placed in blender, is stirred and is stood 30s, obtain seed liquor；Again according to parts by weight, 50 parts are weighed respectively
Deionized water, 2 parts of cetyl trimethylammonium bromides and 2 parts of 0.1mol/L ascorbic acid solutions are placed in a beaker, and are stirred
And pH to 7.0 is adjusted, it is stirred to obtain matrix reaction solution, in 1:5 in mass ratio, seed liquor is added dropwise in matrix reaction solution,
It is stirred and collects and be placed in ultrasonic disperse 15min under 300W, slurries and 1:2 in mass ratio must be dispersed, by dispersion slurries and again
Close sol solutions be stirred juxtaposition still aging 5h at room temperature, collect compound ageing liquid be placed at 50 DEG C rotate be evaporated to
It is dry, it collects dry colloidal sol and is placed in tube-type atmosphere furnace, lead to nitrogen and exclude air, it is 30mL/min that control nitrogen, which is passed through rate,
900 DEG C are warming up to after the completion of being passed through, then by 5 DEG C/min, calcining materials are calcined and collected in heat preservation, and standing is cooled to room temperature and grinds
Honed 200 mesh obtains modified composite Nano Argent grain；According to parts by weight, 50 parts of neopelexes, 50 parts are weighed respectively
Deionized water, 5 parts of 5% poly-vinyl alcohol solutions of mass fraction and 8 parts of composite Nano Argent grains are placed in blender, are stirred simultaneously
It uses diluent to be adjusted to solid content as 70%, the electrochemically resistant migration-type nano silver composite solder paste material can be prepared into
Material.The diluent is preferably terpinol.
Embodiment is tested for the property, specific test result is as follows shown in table table 1:
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Solder melt temperature/DEG C | 558 | 558 | 559 |
| It is sintered layer resistivity/μ Ω cm | 5.68 | 5.24 | 5.01 |
| Jointing shearing strength is at/260 DEG C (MPa) | 45.8 | 45.9 | 45.9 |
As shown in Table 1, solder paste material prepared by the present invention has excellent bonding strength and ability of resisting to migration.
Claims (9)
1. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material, it is characterised in that specific preparation step
Are as follows:
(1) according to parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of 8% poly-vinyl alcohol solutions of mass fraction,
10~15 parts of palladium chloride solutions, 15~20 parts of nickel chloride solutions are placed in conical flask, are led to nitrogen and are excluded air again in nitrogen gas
Insulated and stirred under atmosphere obtains reaction solution and in mass ratio 1:25, and 2% boron hydracid sodium solution of mass fraction is added dropwise in reaction solution,
It is stood after insulation reaction, obtains complex sol liquid；
(2) according to parts by weight, it is molten that 45~50 parts of deionized waters, the sour sodium of 10~15 parts of 10% lemons of mass fraction three are weighed respectively
Liquid, 3~5 parts of 1% nitric acid of mass fraction and 1~2 part of 1% boron hydracid sodium solution of mass fraction are placed in blender, are stirred
And 25~30s is stood, obtain seed liquor；
(3) again according to parts by weight, 45~50 parts of deionized waters, 1~2 part of cetyl trimethylammonium bromide and 1 are weighed respectively
~2 parts of 0.1mol/L ascorbic acid solutions are placed in a beaker, and are stirred and adjust pH to 7.0, are stirred to obtain matrix reaction
Seed liquor is added dropwise in matrix reaction solution by liquid in 1:5 in mass ratio, is stirred and ultrasonic disperse, must disperse slurries and by
Mass ratio 1:2, will dispersion slurries and complex sol liquid to be stirred juxtaposition still aging at room temperature, collect to obtain compound ageing liquid
And rotary evaporation is handled, and collects dry colloidal sol；
(4) dry colloidal sol is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, after the completion of being passed through, heating heating, heat preservation is forged
Calcining materials are burnt and collect, standing is cooled to room temperature and is ground up, sieved, and obtains modified composite Nano Argent grain；According to parts by weight,
It is molten that 45~50 parts of neopelexes, 45~50 parts of deionized waters, 3~5 parts of 5% polyvinyl alcohol of mass fraction are weighed respectively
Liquid and 6~8 parts of composite Nano Argent grains are placed in blender, are stirred and are adjusted using dilution dilution agent, can be prepared into
The electrochemically resistant migration-type nano silver composite solder paste material.
2. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: it is 25~30mL/min that the nitrogen, which is passed through rate,.
3. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the insulated and stirred temperature is 0~5 DEG C.
4. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: it is 1.0~1.5mL/min that drop rate, which is added dropwise, in the 2% boron hydracid sodium solution of amount score.
5. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the rotary evaporation processing is rotary evaporated to dryness at 45~50 DEG C.
6. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the nickel chloride solution is 1:15 in mass ratio, and nickel chloride is added in deionized water, chlorination is stirred to obtain
Nickel solution.
7. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the palladium chloride solution is 1:15 in mass ratio, and palladium chloride is added in deionized water, chlorination is stirred to obtain
Palladium solution.
8. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the diluent is preferably terpinol.
9. a kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material according to claim 1, special
Sign is: the dilution is adjusted to be adjusted to solid content with diluent to be 70%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109433225A (en) * | 2018-08-24 | 2019-03-08 | 北京镭硼科技有限责任公司 | A kind of preparation method and application of the grapheme material of palladium/nickel alloy load |
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| JPS59141395A (en) * | 1983-01-31 | 1984-08-14 | Mitsui Eng & Shipbuild Co Ltd | Brazing filler material |
| CN101745752A (en) * | 2009-12-17 | 2010-06-23 | 北京有色金属研究总院 | Nanometer reinforced bismuth base lead-free high-temperature solder and preparation method thereof |
| US20130160902A1 (en) * | 2011-12-21 | 2013-06-27 | Jun-Der LEE | Manufacturing method for composite alloy bonding wire |
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| CN107511602A (en) * | 2017-08-14 | 2017-12-26 | 武汉工程大学 | A kind of nanometer Ag Cu soldering paste and preparation method and application |
| CN107538148A (en) * | 2017-08-14 | 2018-01-05 | 武汉工程大学 | A kind of composite Nano silver paste and its application |
| CN108555428A (en) * | 2018-05-29 | 2018-09-21 | 北京交通大学 | A kind of preparation method and application of metal-based nano composite solder |
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