CN101767198A - Method for cladding modified lead-free solder alloy powder - Google Patents
Method for cladding modified lead-free solder alloy powder Download PDFInfo
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- CN101767198A CN101767198A CN 201010126840 CN201010126840A CN101767198A CN 101767198 A CN101767198 A CN 101767198A CN 201010126840 CN201010126840 CN 201010126840 CN 201010126840 A CN201010126840 A CN 201010126840A CN 101767198 A CN101767198 A CN 101767198A
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Abstract
The invention discloses a method for cladding modified lead-free solder alloy powder. The method comprises the following steps: selecting superfine SnAgCu or SnInAg or InAg lead-free solder alloy powder, and ultrasonically shaking the powder by adopting an ultrasonic unit which uses alcohol as a medium for 10 to 20 minutes; adding stearic acid into the solution to ensure that the solution is formed to 0.0005 to 0.01mol/L stearic acid alcoholic solution at the temperature of between 50 and 70 DEG C, and preserving the heat for 15 to 45 minutes; separating the cladded alloy powder and the solution through isothermal heat filtration of between 50 and 70 DEG C; and drying the filtered alloy powder in vacuum at the temperature of between 30 and 40 DEG C for 1 to 2 hours to obtain compactly cladded modified solder alloy powder with the thickness between 5 and 10nm. The method ensures that a stearic acid monomolecular or polymolecular layer can be cladded on the surface of the SnAgCu or SnInAg or InAg lead-free solder alloy powder, isolates the alloy powder from environmental medium, and improves the oxidation resistance of the powder, simultaneously the dispersibility and flowability of the solder powder, and the compatibility of the solder alloy powder and organic soldering flux.
Description
Technical field
The invention belongs to the protective layer preparation in surface installation technique field, relate in particular to the surface modification of alloy powder.
Background technology
For a long time, the Sn-Pb scolder becomes the solder of extensive use with convenience, the stability of welding, the rationality of prices of its use.But the use of Pb causes great pollution to environment, has had a strong impact on human beings'health.Scolder unleaded imperative.Europe WEEE and China Ministry of Information Industry have all formulated relevant decree rules, clearly forbid and limit the use of tin-lead solder.
The surface installation technique especially development of flip chip technology (fct) makes that the application in electronics industry of soldering paste is more extensive.On the one hand, thin space, highdensity surface installation technique require to adopt the littler ultra micro solder alloy powder of granularity, to ensure its printing.On the other hand, welding spot size is more and more littler, and the mechanics of its carrying, electricity and thermodynamics load are increasing, reliability requirement is also improved day by day, thereby the quality of soldering paste is had higher requirement.Therefore, surface installation technique needs high-quality meticulous soldering paste.
Metal spontaneous oxidation in surrounding medium or wet environment forms oxide-film, and metal dust is owing to its flourishing specific area, and the surface is easy to oxidation.Be exposed to the oxidation that promptly causes the surface in the air after the solder alloy powder preparation.After being made into soldering paste, welding powder causes soldering paste viscosity to increase also together with the auxiliary agent reaction, and printing performance descends.In auxiliary agent, strengthen active agent content, when welding, can effectively remove oxide-film, but can cause that more postwelding is residual, quicken the corrosion of weld zone.Meet the eco-friendly washing of development trend and exempt from cleaning additive and then can not remove surface film oxide fully.During welding, the welding powder of oxidation not exclusively melts, and separates with oxidation scolder not, rests on the solder joint top layer, perhaps postpones fusing, forms soldered ball.The generation of soldered ball causes the lead short circuit, and weld strength reduces, the obfuscation of solder joint outward appearance.Therefore, the oxidation of welding powder, soldering paste has a strong impact on printing, welding performance and reliability, worsens the soldering paste quality, has also limited its holding time, has seriously restricted its useful life.The lead-free solder alloy powder of ultra-fine granularity has more flourishing specific area, and the surface is easier to oxidation, and is bigger to the welding Effect on Performance.
US5328522(Jul.12,1994) report: the method by cracking, vapour deposition coats paraxylene on the solder alloy powder surface, improves the antioxygenic property of welding powder, and the reflux characteristic of scolder is not produced obviously influence.Yet paraxylene has little toxicity and cladding process complexity.SungilCho etc. are at JOM(2005, and (6): 50-52) go up report: in 150 ℃ of dry state air, the SnZnBi alloy generates ZnO and SnO2, and the existence of Zn impels SnO
2Formation, reduced its non-oxidizability.TIwasaki etc. are at JournalofElectronicMaterials(2005, and 34 (5): 647-654) go up report: the method that adopts ten dihydroxylated acids to pass through the dry state ball milling coats Sn
8Zn
3The Bi welding powder, wettability after cladding powder is deposited and soldered ball experiment show that its antioxygenic property is good.Tan Mu elder sisters etc. are at electronic component and material (2008,27 (2): 45-47) go up report: at ambient temperature, adopt the organic matter C modification Sn of liquid phase method with 2wt%
8Zn
3Bi finds that the modified powder wetability increases, and the speed that the modified powder wettability after the storage reduces is slower.Fei-YiHuang etc. are at JournalofAlloysandCompounds(2006,415:85 – 92) go up report: Sn-3.5Ag-(2.0Cu) solder powder surface film oxide is by SnO and SnO
2Form superficial layer SnO
2Concentration greater than the concentration of SnO, the inner SnO concentration of scolder progressively increases, whole oxidated layer thickness is about 1um.
Summary of the invention
The present invention aims to provide a kind of new SnAgCu or the surface modifying method of SnInAg or InAg lead-free solder alloy powder, to improve these lead-free solder alloy powder antioxygenic properties, prolongs memory time, and improves the mobile and dispersed of solder alloy powder.
The detailed technology scheme of the surface modifying method of lead-free solder alloy powder of the present invention is: get fine SnAgCu or SnInAg or InAg lead-free solder alloy powder, adopting with alcohol is the ultrasonic vibrations 10 ~ 20min of Ultrasound Instrument of medium; It is the stearic acid alcoholic solution of 0.0005-0.01mol/L that the adding stearic acid makes it form concentration in the time of 50 ~ 70 ℃, and is incubated 15 ~ 45min; Separate clad alloy powder and solution through warm suction filtrations such as 50 ~ 70 ℃; Alloy powder got final product to such an extent that thickness is 5 ~ 10nm, the modification solder alloy powder that coats densification in 1 ~ 2 hour through 30 ~ 40 ℃ of vacuum drying behind the suction filtration.
In the method, employing is that the purpose of the ultrasonic vibrations lead-free solder alloy powder of Ultrasound Instrument of medium is to remove surperficial adsorbed gas and oxide-film as far as possible with alcohol.Alloy powder is being incubated 15-45min in the stearic acid alcoholic solution at 0.0005-0.01mol/L under the 50-70 ℃ of temperature, the stearic acid molecule through the isothermal absorption-desorption attached-again absorption physical process, just be coated on the solder alloy powder surface, form surperficial unimolecule or polymolecular adsorption layer.
Use method of modifying of the present invention, coated stearic acid unimolecule or polymolecular layer, isolated alloy powder and surrounding medium, improved the antioxygenic property of powder at SnAgCu or SnInAg or InAg lead-free solder alloy powder surface.Experimental result shows, the SnAgCu or SnInAg or the InAg lead-free solder alloy powder that coat with the inventive method, storage after 9 months in the normal temperature wet environment, the oxygen content increment of cladding powder only be approximately not cladding powder 40%.Simultaneously, because the alloy powder surface forms stearic acid unimolecule or polymolecular layer, can also change the powder surface hydrophilic lipophilic balance like this, thereby improved the dispersed and mobile of welding powder, improved the compatibility of solder alloy powder and organic scaling powder, and improved the stability of soldering paste, optimized the soldering paste serviceability.Therefore says to have good non-oxidizability with the modified alloy powder of the inventive method acquisition, and good dispersion, good fluidity can improve the wetability and the stability of soldering paste.
Description of drawings
Fig. 1 is the TEM figure of the SnAgCu solder alloy powder of embodiment 1 coating modification.
The specific embodiment
Embodiment 1Take by weighing the fine SnAgCu solder alloy powder of 5g; With alcohol is medium, adopts the ultrasonic vibrations solder alloy powder of Ultrasound Instrument 10min, removes the gas and the oxide-film of alloy powder surface absorption; Adding an amount of stearic acid, to make it form concentration in the time of 60 ℃ be the stearic acid alcoholic solution of 0.01mol/L; At 60 ℃ of following insulation 15min, the stearic acid molecule through the isothermal absorption-desorption attached-physical process of absorption again is coated on SnAgCu solder alloy powder surface, forms surperficial bimolecular adsorption layer; Adopt the hot nutsch filter of decompression, separate alloy powder and the solution that coats through warm suction filtrations such as 60 ℃; After 2 hours, acquisition thickness is 5-10nm, the modification solder alloy powder that coats densification to alloy powder through 40 ℃ of vacuum drying behind the suction filtration.
The TEM figure of obtained product sees accompanying drawing 1.Adopt the method at powder maximum stable angle in the rotary drum to test the result: coat and clad alloy powder maximum stable angle is respectively 69.43 °, 66.50 °, with respect to cladding powder not, cladding powder has better flowability; Storage is after 9 months in the normal temperature wet environment, and the oxygen content increment of cladding powder is 0.0349wt%, and cladding powder oxygen content increment is not 0.0723wt%, and therefore, the antioxygenic property of modified powder obviously is better than unmodified powder.
Embodiment 2Taking by weighing the fine SnInAg solder alloy powder of 3g, is medium with alcohol, adopts the ultrasonic vibrations solder alloy powder of Ultrasound Instrument 15min, removes the gas and the oxide-film of alloy powder surface absorption; It is the stearic acid alcoholic solution of 0.001mol/L that the adding stearic acid makes it form concentration in the time of 60 ℃; At 60 ℃ of following insulation 30min, the stearic acid molecule through the isothermal absorption-desorption attached-physical process of absorption again is coated on SnInAg solder alloy powder surface, forms surperficial bimolecular adsorption layer; Adopt the hot nutsch filter of decompression, separate alloy powder and the solution that coats through warm suction filtrations such as 60 ℃, after 1 hour, acquisitions thickness is 5-10nm, the modification solder alloy powder that coats densification to alloy powder through 30 ℃ of vacuum drying behind the suction filtration.
Claims (3)
1. the method for a cladding modified lead-free solder alloy powder is got fine SnAgCu or SnInAg or InAg lead-free solder alloy powder, and adopting with alcohol is the ultrasonic vibrations 10 ~ 20min of Ultrasound Instrument of medium; It is the stearic acid alcoholic solution of 0.0005-0.01mol/L that the adding stearic acid makes it form concentration, and is incubated 15 ~ 45min; Separate clad alloy powder and solution through warm suction filtrations such as 50 ~ 70 ℃; Alloy powder got final product through SnAgCu or the SnInAg or the InAg lead-free solder alloy powder of modification in 1 ~ 2 hour through 30 ~ 40 ℃ of vacuum drying behind the suction filtration.
2. the method for claim 1, it is characterized in that: described adding stearic acid makes it form the alcoholic solution of 0.0005-0.01mol/L in the time of 60 ℃.
3. modification SnAgCu or the SnInAg or the InAg lead-free solder alloy powder of method preparation as claimed in claim 1 or 2 is characterized in that the stearic acid thickness that coats is 5 ~ 10nm.
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| CN2010101268404A CN101767198B (en) | 2010-03-18 | 2010-03-18 | Method for cladding modified lead-free solder alloy powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103221164A (en) * | 2010-11-18 | 2013-07-24 | 同和控股（集团）有限公司 | Solder powder and process for producing solder powder |
| CN103619529A (en) * | 2011-09-02 | 2014-03-05 | 三菱综合材料株式会社 | Solder powder, and solder paste using solder powder |
| CN105772711A (en) * | 2016-04-27 | 2016-07-20 | 攀枝花学院 | Surface treatment method of titanium powder and titanium alloy powder for sintering |
| CN107214431A (en) * | 2017-07-12 | 2017-09-29 | 北京康普锡威科技有限公司 | A kind of normal temperature storage is combined tin cream and preparation method |
| CN112238223A (en) * | 2019-07-18 | 2021-01-19 | 上栗县科源冶金材料有限公司 | Anti-oxidation method for storing metal powder |
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| CN1839000A (en) * | 2003-07-09 | 2006-09-27 | 福莱金属公司 | Coating metal particles |
| CN1895838A (en) * | 2005-07-12 | 2007-01-17 | 北京有色金属研究总院 | Sn-Ag-Cu-Cr-X lead-free soldering material and its preparation |
| KR20090084092A (en) * | 2008-01-31 | 2009-08-05 | 한양대학교 산학협력단 | Method of fabricating iron nano powder sintered part |
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2010
- 2010-03-18 CN CN2010101268404A patent/CN101767198B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1839000A (en) * | 2003-07-09 | 2006-09-27 | 福莱金属公司 | Coating metal particles |
| CN1895838A (en) * | 2005-07-12 | 2007-01-17 | 北京有色金属研究总院 | Sn-Ag-Cu-Cr-X lead-free soldering material and its preparation |
| KR20090084092A (en) * | 2008-01-31 | 2009-08-05 | 한양대학교 산학협력단 | Method of fabricating iron nano powder sintered part |
Non-Patent Citations (1)
| Title |
|---|
| 《功能材料》 20100131 刘文胜等 真空蒸镀硬脂酸包覆SnAgCu无铅焊料合金粉末研究 144-147，152 3 第41卷, 第1期 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103221164A (en) * | 2010-11-18 | 2013-07-24 | 同和控股（集团）有限公司 | Solder powder and process for producing solder powder |
| CN103221164B (en) * | 2010-11-18 | 2016-06-15 | 同和控股（集团）有限公司 | The manufacture method of solder powder and solder powder |
| CN103619529A (en) * | 2011-09-02 | 2014-03-05 | 三菱综合材料株式会社 | Solder powder, and solder paste using solder powder |
| US8882934B2 (en) | 2011-09-02 | 2014-11-11 | Mitsubishi Materials Corporation | Solder powder, and solder paste using solder powder |
| CN105772711A (en) * | 2016-04-27 | 2016-07-20 | 攀枝花学院 | Surface treatment method of titanium powder and titanium alloy powder for sintering |
| CN105772711B (en) * | 2016-04-27 | 2018-05-11 | 攀枝花学院 | The surface treatment method of sintering titanium valve and titanium alloy powder |
| CN107214431A (en) * | 2017-07-12 | 2017-09-29 | 北京康普锡威科技有限公司 | A kind of normal temperature storage is combined tin cream and preparation method |
| CN107214431B (en) * | 2017-07-12 | 2020-06-16 | 北京康普锡威科技有限公司 | Normal-temperature storage composite solder paste and preparation method thereof |
| CN112238223A (en) * | 2019-07-18 | 2021-01-19 | 上栗县科源冶金材料有限公司 | Anti-oxidation method for storing metal powder |
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| CN101767198B (en) | 2011-11-30 |
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