CN109352206A - A kind of alloy nanoparticle soldering paste and preparation method thereof - Google Patents
A kind of alloy nanoparticle soldering paste and preparation method thereof Download PDFInfo
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- CN109352206A CN109352206A CN201811370679.8A CN201811370679A CN109352206A CN 109352206 A CN109352206 A CN 109352206A CN 201811370679 A CN201811370679 A CN 201811370679A CN 109352206 A CN109352206 A CN 109352206A
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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
- 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
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to nanotechnologies and microelectronics Packaging field, and disclose a kind of alloy nanoparticle soldering paste and preparation method thereof.This method specific steps are as follows: metal salt and stabilizer are dissolved completely in solvent, metal salt solution is made, reducing agent is added in the metal salt solution and stirs, reacted it sufficiently and obtain alloy nanoparticle suspension；It is separated by solid-liquid separation alloy nanoparticle suspension to obtain sediment, washs the sediment using cleaning agent, it is then dry to obtain alloy nanoparticle；Alloy nanoparticle is added in organic thickening agent, by being stirred under vacuum with after de-bubble processing, alloy nanoparticle soldering paste is made.The present invention prepares alloy nanoparticle using liquid phase reduction, and simple process, easily controllable and cost is relatively low；Stabilizer is added when preparing metal salt solution, can effectively avoid the reunion and oxidation of particle, enhance the inoxidizability of alloy nanoparticle.
Description
Technical field
The invention belongs to nanotechnologies and microelectronics Packaging field, more particularly, to a kind of alloy nanoparticle soldering paste
And preparation method thereof.
Background technique
With electronic device densification, high power and the continuous development of micromation, heat-resisting quantity to solder and
The performances such as stability in use propose more harsh requirement.Although leaded high-temperature solder has good high temperature resistance, and
Be widely used in Electronic Packaging field, but solder containing pb to environmental and human health impacts there are serious harm, do not meet energy-saving ring
Protect the development trend with green manufacturing.And although developed lead-free solder is avoided that the use of solder containing pb, but still exist
More disadvantage, such as bismuthino solder embrittlement is big, zinc-base solder is not corrosion-resistant and the high cost of auri solder etc..In addition, these solders
Layer easily occur at high temperature tin reflux and thermal stress it is excessive and the case where cause short circuit to fail, it is difficult to guarantee power electronic device
Part long term reliability.Therefore, develop a kind of function admirable inexpensive lead-free solder be microelectronics Packaging field urgently
The technical problem of solution.
In recent years, metal nanoparticle soldering paste not only has good conductivity and thermal conductivity, but also is able to achieve low temperature key
The target with high-temperature service is closed, the extensive concern of academia and industry is caused, provides a kind of new skill for microelectronics Packaging
Art route.Patent of invention CN201010301224.8, CN201010301221.4, CN201010301190.2 pass through addition respectively
Nickel, iron and silver nano-grain enhance the plasticity of unleaded tinol, inhibit growing up for welding point interface intermetallic compound, to mention
Strong mechanical performance and stability, but the problems such as tin reflux and electromigration are not resolved under high temperature.
Currently, silver and copper nano particles soldering paste rely on its high conductivity and thermal conductivity, sintering temperature and low and excellent mechanical property
The advantages such as energy become the focus and emphasis of nano leadless soldering paste research.But silver and copper nano particles soldering paste all exist it is some can not
The expensive and anti-ion transport of the defect avoided, such as silver is poor, and copper nano particles easily aoxidize, and oxide on surface can be significant
Increase sintering temperature and reduces conductivity.There is researcher by preparing core shell nanoparticles (copper-silver, copper-nickel and copper-tin) to press down
The oxidation of copper nano particles processed, but this core-shell structure preparation process is complicated, and core-shell structure generates mutually separate at high temperature
Also it will further decrease conductivity；On the other hand, alloy nanoparticle can balance the advantage and disadvantage of various metals well, such as copper-
Silver alloy nano particle not only has good thermal conductivity and conductivity, and has good inoxidizability and anti-Ion transfer
Performance.
Summary of the invention
For the disadvantages mentioned above and/or Improvement requirement of the prior art, the present invention provides a kind of alloy nanoparticle soldering paste
And preparation method thereof, wherein the preparation method should be able to mutually be effectively reduced by the way that stabilizer is added when preparing metal salt solution
The generation of agglomeration and oxidation reaction during alloy nanoparticle is prepared, so that the alloy nanoparticle soldering paste of preparation is especially
Suitable for application fields such as microelectronics Packaging and three dimensional integrated circuits.
To achieve the above object, according to one aspect of the present invention, a kind of preparation of alloy nanoparticle soldering paste is proposed
Method, which is characterized in that this method comprises the following steps:
(a) metal salt and stabilizer are dissolved completely in solvent and metal salt solution is made, added in the metal salt solution
Enter reducing agent and stir, reacts it sufficiently and obtain alloy nanoparticle suspension；
(b) it is separated by solid-liquid separation alloy nanoparticle suspension obtained in step (a) to obtain sediment, utilizes cleaning
The sediment is washed in agent, and is dried acquisition alloy nanoparticle；
(c) alloy nanoparticle obtained in step (b) is added in organic thickening agent, passes through vacuum stirring and de-bubble
After processing, alloy nanoparticle soldering paste is made.
As it is further preferred that in the step (a) cation of metal salt be preferably copper ion, silver ion, tin from
Son and nickel ion in it is any two or more；The anion of the metal salt is preferably chloride ion, bromide ion, nitrate anion
One of ion, sulfate ion, formate ion and acetate ion are a variety of.
As it is further preferred that stabilizer is preferably oleyl amine, oleic acid, polyvinylpyrrolidone, ten in the step (a)
One of dialkyl sulfonates, resin, mercaptan type organic, amide type organic and hydramine type organic are a variety of；Solvent
Preferably one of deionized water, ethylene glycol, ethyl alcohol, diethylene glycol, glycerine, 1,2-PD and pentanediol or more
Kind；Reducing agent is preferably one of hydrazine hydrate, phenylhydrazine, sodium borohydride, sodium citrate and sodium hypophosphite or a variety of.
As it is further preferred that metal salt and stabilizer are preferably mixed with the molar ratio of 1:2~1:30 in the step (a)
It closes, and is further preferably mixed with the molar ratio of 1:10~1:20；Metal salt and reducing agent are preferably with the molar ratio of 1:2~1:15
Mixing, and further preferably mixed with the molar ratio of 1:5~1:10.
As it is further preferred that mixing time is preferably 0.5h~for 24 hours in the step (a), whipping temp is preferably 5
DEG C~100 DEG C.
As it is further preferred that cleaning agent is preferably deionized water, methanol, dehydrated alcohol, third in the step (b)
One of alcohol, n-butanol, pentane, hexane, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide and toluene are a variety of.
As it is further preferred that drying temperature is preferably 60 DEG C~80 DEG C in the step (b), drying time is preferably
2h~12h, the partial size of alloy nanoparticle obtained are preferably 5nm~300nm.
As it is further preferred that organic thickening agent is preferably methocel solution, ethyl cellulose in the step (c)
One of plain solution, hydroxyethyl cellulose solution, terpinol, isopropanol, polyethylene glycol, polyvinyl acetate and glycerine or
It is a variety of.
As it is further preferred that alloy nanoparticle in alloy nanoparticle soldering paste obtained in the step (c)
Mass percent is preferably 70%~95%.
It is another aspect of this invention to provide that providing a kind of alloy nanoparticle soldering paste prepared using the above method.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1. the present invention prepares alloy nanoparticle using liquid phase reduction, this method has simple process, technological parameter easy
In control, the technical advantages such as cost is relatively low；
2. especially, stabilizer is added when preparing metal salt solution by the present invention, it is made to be coated on alloy nanoparticle table
Face, or coordinate bond is formed with metal ion, the reunion of particle can be effectively avoided, keeps the particle diameter distribution of alloy nanoparticle equal
It is even, there is good dispersibility, saved for it and use provides advantageous condition；Meanwhile the stabilizer of addition can also have
Effect inhibits the oxidation of alloy nanoparticle, finds after being characterized as the alloy nanoparticle to made from, has apparent
Metal simple-substance diffraction maximum illustrates that the alloy nanoparticle has good antioxygen without the diffraction maximum of the impurity such as metal oxide
The property changed is particularly suitable for the technical fields such as low temperature interconnection and microelectronics Packaging；
3. molar ratio of the present invention by setting metal salt and stabilizer can guarantee alloy obtained as 1:2~1:30
The partial size of nano particle in the range of 5nm~300nm, and can according in actual use to alloy nanoparticle partial size
Demand selects suitable molar ratio, guarantees that avoiding being added excessive stabilizer while using effect increases production cost；Simultaneously
The present invention also sets the molar ratio of metal salt and reducing agent as 1:2~1:15, can guarantee that metal ion is reduced to gold completely
Belong to simple substance, reinforces the inoxidizability of the alloy nanoparticle of preparation；
4. simultaneously, alloy nanoparticle prepared by the present invention has the spy of significant small-size effect and high apparent activation energy
Point, to realize that the target of low-temperature sintering and high-temperature service provides highly beneficial condition；
5. in addition, alloy nanoparticle prepared by the present invention with two kinds or two kinds in mantoquita, silver salt, pink salt, nickel salt with
Upper metal salt efficiently solves the problems, such as that active metal is oxidizable and heavy metal is high-cost, greatly extends conjunction as raw material
The application range of gold nano grain.
Detailed description of the invention
Fig. 1 is the preparation flow figure of alloy nanoparticle solder provided by the invention；
Fig. 2 is the XRD spectrum of the alloy nanoparticle HJ-1 prepared in the embodiment of the present invention 1；
Fig. 3 is the TEM figure of the alloy nanoparticle HJ-2 prepared in the embodiment of the present invention 2；
Fig. 4 is the XPS map of the alloy nanoparticle HJ-2 prepared in the embodiment of the present invention 2.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
The invention proposes a kind of preparation method of alloy nanoparticle soldering paste, preparation flow is as shown in Figure 1, specific packet
Include following steps:
(a) metal salt and stabilizer are dissolved completely in solvent and metal salt solution is made, added in the metal salt solution
Enter reducing agent and stir, reacts it sufficiently and obtain alloy nanoparticle suspension；
(b) alloy nanoparticle suspension obtained in step (a) is preferably separated by solid-liquid separation using the method for centrifugation
Sediment is obtained, washs the sediment using cleaning agent, and be dried acquisition alloy nanoparticle；
(c) alloy nanoparticle obtained in step (b) is added in organic thickening agent, passes through vacuum stirring and de-bubble
After processing, alloy nanoparticle soldering paste is made.
Further, the cation of metal salt is preferably copper ion, silver ion, tin ion and nickel ion in the step (a)
In it is any two or more；The anion of the metal salt is preferably chloride ion, bromide ion, nitrate ion, sulfuric acid
One of radical ion, formate ion and acetate ion are a variety of.
Further, stabilizer is preferably oleyl amine, oleic acid, polyvinylpyrrolidone, dodecyl sodium sulfonate in the step (a)
One of sodium, resin, mercaptan type organic, amide type organic and hydramine type organic are a variety of；Solvent preferably go from
One of sub- water, ethylene glycol, ethyl alcohol, diethylene glycol, glycerine, 1,2-PD and pentanediol are a variety of；Reducing agent is excellent
It is selected as one of hydrazine hydrate, phenylhydrazine, sodium borohydride, sodium citrate and sodium hypophosphite or a variety of.
Further, metal salt is preferably mixed with stabilizer with the molar ratio of 1:2~1:30 in the step (a), goes forward side by side one
Step is preferably mixed with the molar ratio of 1:10~1:20；Metal salt is preferably mixed with reducing agent with the molar ratio of 1:2~1:15, is gone forward side by side
One step is preferably mixed with the molar ratio of 1:5~1:10.
Further, mixing time is preferably 0.5h~for 24 hours in the step (a), and whipping temp is preferably 5 DEG C~100 DEG C.
Further, cleaning agent is preferably deionized water, methanol, dehydrated alcohol, propyl alcohol, n-butanol, penta in the step (b)
One of alkane, hexane, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide and toluene are a variety of.
Further, drying temperature is preferably 60 DEG C~80 DEG C in the step (b), and drying time is preferably 2h~12h, system
The partial size of the alloy nanoparticle obtained is preferably 5nm~300nm.
Further, organic thickening agent is preferably methocel solution, ethyl cellulose solution, hydroxyl in the step (c)
One of ethyl cellulose solution, terpinol, isopropanol, polyethylene glycol, polyvinyl acetate and glycerine are a variety of.
Further, in the step (c) in alloy nanoparticle soldering paste obtained alloy nanoparticle mass percent
Preferably 70%~95%.
Further the present invention is specifically described with specific embodiment below.
Embodiment 1
(a) it using copper formate and silver acetate as metal salt, is dissolved completely in ethylene glycol and is made after being mixed with isopropanolamine
Then reducing agent hydrazine hydrate is added in the metal salt solution and is continuously stirred at room temperature 24 hours, makes it for metal salt solution
Sufficiently reaction obtains alloy nanoparticle suspension, and wherein the molar ratio of metal salt and isopropanolamine is 1:10, metal salt and water
The molar ratio of hydrazine is closed as 1:10, the molar ratio of copper formate and silver acetate is 4:1；
(b) it is centrifuged alloy nanoparticle suspension obtained in step (a) to obtain sediment, utilizes N, N- diformazan
Yl acetamide and toluene successively carry out carrying out washing treatment to it, and vacuum drying 2 hours is then carried out at 80 DEG C, obtain partial size and are
The alloy nanoparticle of 50nm~200nm, is denoted as HJ-1；
(c) HJ-1 obtained in step (b) is added in glycerine, by being stirred under vacuum with after de-bubble processing, is made
Alloy nanoparticle soldering paste, wherein the mass percent of HJ-1 is 80%.
XRD test is carried out to HJ-1 obtained, obtains map as shown in Fig. 2, to contain only Cu in the alloy nanoparticle mono-
The diffraction maximum of matter and Ag simple substance, without the diffraction maximum of other substances such as metal oxide, it was demonstrated that prepared using method of the invention
Alloy nanoparticle have good inoxidizability.
Embodiment 2
(a) it using copper acetate and silver acetate as metal salt, is dissolved completely in ethylene glycol and is made after being mixed with isopropanolamine
Then reducing agent sodium borohydride is added in the metal salt solution and persistently stirs 6 hours at 5 DEG C, makes it for metal salt solution
Sufficiently reaction obtains alloy nanoparticle suspension, and wherein the molar ratio of metal salt and isopropanolamine is 1:20, metal salt and boron
The molar ratio of sodium hydride is 1:8, and the molar ratio of copper acetate and silver acetate is 7:3；
(b) it is filtered alloy nanoparticle suspension obtained in step (a) to obtain sediment, using pentane to it
Carrying out washing treatment is carried out, vacuum drying 8 hours is then carried out at 70 DEG C, obtains the alloy nano that partial size is 5nm~100nm
Grain, is denoted as HJ-2；
(c) HJ-2 obtained in step (b) is added in ethylene glycol, by being stirred under vacuum with after de-bubble processing, is made
Alloy nanoparticle soldering paste, wherein the mass percent of HJ-2 is 70%.
TEM test is carried out to HJ-2 obtained, as a result as shown in figure 3, agglomeration does not occur in the alloy nanoparticle,
And partial size is between 5nm~100nm, is distributed more uniform, it was demonstrated that the present invention by stabilizer is added it is possible to prevente effectively from
Grain is reunited, and the partial size of alloy nanoparticle can be controlled by the adding proportion of regulating stabilizer；
XPS test is carried out to HJ-2 obtained simultaneously, as a result as shown in figure 4, in the XPS map of the alloy nanoparticle only
There is the diffraction maximum of Cu simple substance and Ag simple substance, not the diffraction maximum of metal oxide, further illustrates using the preparation in the present invention
Alloy nanoparticle made from method has good inoxidizability.
Embodiment 3
(a) using tin tetrachloride, copper acetate and silver nitrate as metal salt, 1,2- the third two is dissolved completely in after mixing with oleic acid
Metal salt solution is made in alcohol, reducing agent sodium borohydride is then added in the metal salt solution and persistently stirs 3 at 60 DEG C
Hour, it reacts it sufficiently and obtains alloy nanoparticle suspension, wherein the molar ratio of metal salt and oleic acid is 1:15, metal salt
Molar ratio with sodium borohydride is 1:5, and the molar ratio of tin tetrachloride, copper acetate and silver nitrate is 1:3:1；
(b) it is centrifuged alloy nanoparticle suspension obtained in step (a) to obtain sediment, using hexane to it
Carrying out washing treatment is carried out, vacuum drying 12 hours is then carried out at 60 DEG C, obtains the alloy nano that partial size is 50nm~200nm
Grain, is denoted as HJ-3；
(c) HJ-3 obtained in step (b) is added in o polyhydroxyethyl cellulose, is handled by being stirred under vacuum with de-bubble
Afterwards, alloy nanoparticle soldering paste is made, wherein the mass percent of HJ-3 is 95%.
Embodiment 4
(a) it using silver chlorate and tin tetrachloride as metal salt, is dissolved completely in after being mixed with oleyl amine in glycerine and gold is made
Belong to salting liquid, reducing agent phenylhydrazine is then added in the metal salt solution and is persistently stirred at 40 DEG C 12 hours, makes it sufficiently
Reaction obtains alloy nanoparticle suspension, and wherein the molar ratio of metal salt and oleyl amine is 1:2, the molar ratio of metal salt and phenylhydrazine
For 1:15, the molar ratio of silver chlorate and tin tetrachloride is 3:1；
(b) it is centrifuged alloy nanoparticle suspension obtained in step (a) to obtain sediment, using hexane to it
Carrying out washing treatment is carried out, vacuum drying 6 hours is then carried out at 75 DEG C, obtains the alloy nano that partial size is 100nm~300nm
Grain, is denoted as HJ-4；
(c) HJ-4 obtained in step (b) is added in o polyhydroxyethyl cellulose, is handled by being stirred under vacuum with de-bubble
Afterwards, alloy nanoparticle soldering paste is made, wherein the mass percent of HJ-4 is 85%.
Embodiment 5
(a) it using copper acetate and nickel sulfate as metal salt, is dissolved completely in ethylene glycol and is made after being mixed with lauryl mercaptan
Then reducing agent sodium citrate is added in the metal salt solution and persistently stirs at 100 DEG C 0.5 hour for metal salt solution,
It reacts it sufficiently and obtains alloy nanoparticle suspension, wherein the molar ratio of metal salt and lauryl mercaptan is 1:30, metal salt
It is 1:2 with the molar ratio of sodium citrate, the molar ratio of copper acetate and nickel sulfate is 2:3；
(b) it is separated by solid-liquid separation alloy nanoparticle suspension obtained in step (a) to obtain sediment, utilization is anhydrous
Ethyl alcohol carries out carrying out washing treatment to it, and vacuum drying 4 hours is then carried out at 65 DEG C, obtains the alloy that partial size is 5nm~100nm
Nano particle is denoted as HJ-5；
(c) HJ-5 obtained in step (b) is added in polyvinyl acetate solution, at vacuum stirring and de-bubble
After reason, alloy nanoparticle soldering paste is made, wherein the mass percent of HJ-5 is 75%.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of alloy nanoparticle soldering paste, which is characterized in that this method comprises the following steps:
(a) metal salt and stabilizer are dissolved completely in solvent and metal salt solution is made, be added also in the metal salt solution
Former agent is simultaneously stirred, and is reacted it sufficiently and is obtained alloy nanoparticle suspension；
(b) it is separated by solid-liquid separation alloy nanoparticle suspension obtained in step (a) to obtain sediment, be washed using cleaning agent
The sediment is washed, and is dried acquisition alloy nanoparticle；
(c) alloy nanoparticle obtained in step (b) is added in organic thickening agent, is handled by being stirred under vacuum with de-bubble
Afterwards, alloy nanoparticle soldering paste is made.
2. the preparation method of alloy nanoparticle soldering paste as described in claim 1, which is characterized in that golden in the step (a)
Belong to salt cation be preferably in copper ion, silver ion, tin ion and nickel ion it is any two or more；The metal
The anion of salt is preferably in chloride ion, bromide ion, nitrate ion, sulfate ion, formate ion and acetate ion
It is one or more.
3. the preparation method of alloy nanoparticle soldering paste as claimed in claim 1 or 2, which is characterized in that in the step (a)
Stabilizer is preferably oleyl amine, oleic acid, polyvinylpyrrolidone, dodecyl sodium sulfate, resin, mercaptan type organic, amides
One of organic matter and hydramine type organic are a variety of；Solvent be preferably deionized water, ethylene glycol, ethyl alcohol, diethylene glycol,
One of glycerine, 1,2-PD and pentanediol are a variety of；Reducing agent is preferably hydrazine hydrate, phenylhydrazine, sodium borohydride, lemon
One of sour sodium and sodium hypophosphite are a variety of.
4. the preparation method of alloy nanoparticle soldering paste as claimed in any one of claims 1 to 3, which is characterized in that the step
Suddenly metal salt is preferably mixed with stabilizer with the molar ratio of 1:2~1:30 in (a), and further preferably rubbing with 1:10~1:20
You are than mixing；Metal salt is preferably mixed with reducing agent with the molar ratio of 1:2~1:15, and further preferably with 1:5~1:10's
Molar ratio mixing.
5. such as the preparation method of the described in any item alloy nanoparticle soldering paste of Claims 1 to 4, which is characterized in that the step
Suddenly mixing time is preferably 0.5h~for 24 hours in (a), and whipping temp is preferably 5 DEG C~100 DEG C.
6. the preparation method of alloy nanoparticle soldering paste as claimed in any one of claims 1 to 5, which is characterized in that the step
Suddenly cleaning agent is preferably deionized water, methanol, dehydrated alcohol, propyl alcohol, n-butanol, pentane, hexane, N, N- dimethyl methyl in (b)
One of amide, DMAC N,N' dimethyl acetamide and toluene are a variety of.
7. the preparation method of alloy nanoparticle soldering paste as described in any one of claims 1 to 6, which is characterized in that the step
Suddenly drying temperature is preferably 60 DEG C~80 DEG C in (b), and drying time is preferably 2h~12h, the grain of alloy nanoparticle obtained
Diameter is preferably 5nm~300nm.
8. the preparation method of alloy nanoparticle soldering paste as described in any one of claims 1 to 7, which is characterized in that the step
Suddenly in (c) organic thickening agent be preferably methocel solution, ethyl cellulose solution, hydroxyethyl cellulose solution, terpinol,
One of isopropanol, polyethylene glycol, polyvinyl acetate and glycerine are a variety of.
9. the preparation method of alloy nanoparticle soldering paste as described in any one of claims 1 to 8, which is characterized in that the step
Suddenly the mass percent of alloy nanoparticle is preferably 70%~95% in alloy nanoparticle soldering paste obtained in (c).
10. a kind of utilize alloy nanoparticle soldering paste made from according to any one of claims 1 to 99 described in any item methods.
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| CN110026567A (en) * | 2019-04-24 | 2019-07-19 | 昶联金属材料应用制品(广州)有限公司 | Silver-copper nano particle and its preparation method and application |
| CN111408870A (en) * | 2020-04-01 | 2020-07-14 | 重庆群崴电子材料有限公司 | Nano bimetal super solid solution structure soldering paste and preparation method thereof |
| CN111408869A (en) * | 2020-04-10 | 2020-07-14 | 华中科技大学 | Micro-nano copper particle soldering paste for low-temperature bonding and preparation method and application thereof |
| CN111715878A (en) * | 2020-07-01 | 2020-09-29 | 西安交通大学 | High-performance composite nano bonding material and preparation method thereof |
| CN112475313A (en) * | 2020-11-11 | 2021-03-12 | 昆明理工大学 | Method for preparing nano-scale solder additive through chemical reaction |
| CN112935240A (en) * | 2021-01-20 | 2021-06-11 | 深圳市先进连接科技有限公司 | Micro-nano composite silver paste, preparation method thereof and packaging method of airtight device |
| CN113102765A (en) * | 2021-04-06 | 2021-07-13 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Copper nano-sphere particle and preparation method and application thereof |
| CN114473110A (en) * | 2022-02-28 | 2022-05-13 | 深圳先进电子材料国际创新研究院 | Electromigration-resistant and oxidation-resistant soldering paste and application thereof |
| CN115302129A (en) * | 2022-08-01 | 2022-11-08 | 中车青岛四方机车车辆股份有限公司 | Tin solder for stainless steel brazing and preparation method of tin solder |
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| CN111408870A (en) * | 2020-04-01 | 2020-07-14 | 重庆群崴电子材料有限公司 | Nano bimetal super solid solution structure soldering paste and preparation method thereof |
| CN111408869A (en) * | 2020-04-10 | 2020-07-14 | 华中科技大学 | Micro-nano copper particle soldering paste for low-temperature bonding and preparation method and application thereof |
| CN111408869B (en) * | 2020-04-10 | 2021-05-18 | 华中科技大学 | Micro-nano copper particle soldering paste for low-temperature bonding and preparation method and application thereof |
| CN111715878A (en) * | 2020-07-01 | 2020-09-29 | 西安交通大学 | High-performance composite nano bonding material and preparation method thereof |
| CN112475313A (en) * | 2020-11-11 | 2021-03-12 | 昆明理工大学 | Method for preparing nano-scale solder additive through chemical reaction |
| CN112935240A (en) * | 2021-01-20 | 2021-06-11 | 深圳市先进连接科技有限公司 | Micro-nano composite silver paste, preparation method thereof and packaging method of airtight device |
| CN113102765A (en) * | 2021-04-06 | 2021-07-13 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Copper nano-sphere particle and preparation method and application thereof |
| CN113102765B (en) * | 2021-04-06 | 2023-07-21 | 中科南京绿色制造产业创新研究院 | Copper nano-sphere particles and preparation method and application thereof |
| CN114473110A (en) * | 2022-02-28 | 2022-05-13 | 深圳先进电子材料国际创新研究院 | Electromigration-resistant and oxidation-resistant soldering paste and application thereof |
| CN114473110B (en) * | 2022-02-28 | 2024-01-26 | 深圳先进电子材料国际创新研究院 | Electromigration-resistant and oxidation-resistant soldering paste and application thereof |
| CN115302129A (en) * | 2022-08-01 | 2022-11-08 | 中车青岛四方机车车辆股份有限公司 | Tin solder for stainless steel brazing and preparation method of tin solder |
| CN115302129B (en) * | 2022-08-01 | 2023-09-15 | 中车青岛四方机车车辆股份有限公司 | Solder paste for stainless steel brazing and preparation method of solder paste |
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Application publication date: 20190219 |