CN101791748A - Sn-Ag-Cu-Zn-Ge lead-free solder for inhibiting solid-state interface reaction and preparation method thereof - Google Patents
Sn-Ag-Cu-Zn-Ge lead-free solder for inhibiting solid-state interface reaction and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an Sn-Ag-Cu-Zn-Ge lead-free solder for inhibiting solid-state interface reaction and a preparation method thereof for the technical field of electronic packaging. The solder comprises the following components in mass percent: 0%-3.5% of Ag, 0%-0.7% of Cu, 0%-2% of Zn, 0%-0.3% of Ge and balance of Sn. The preparation method comprises the following steps: firstly, putting Sn particles into a KCl and LiCl eutectic protection salt solution, heating, adding high-purity Ag wires and/or Cu wires, insulating for the first time, and fully stirring to obtain a uniform Sn-TM solution; then, adding trace Zn foil and/or Ge particles into the alloy solution, insulating for the second time, and fully stirring; and cooling and pouring the solution into a solder mold. The invention solves the problems that in the prior art, because the lead-free solder has high Sn content, the lead-free solder can react with substrate metals easily, thereby causing a large amount of substrates to be dissolved, and simultaneously, a large amount of intermetallic compounds are formed on the interface, thereby seriously influencing the reliability of the interface. The lead-free solder of the invention has simple preparation processes and can be prepared in batch easily.
Description
Technical field
What the present invention relates to is a kind of solder that is used for technical field of electronic encapsulation and preparation method thereof, a kind of specifically Sn-Ag-Cu-Zn-Ge lead-free brazing that suppresses solid-state interfacial reaction and preparation method thereof.
Technical background
SnPb is traditional electronic package material, because Pb threatens natural environment and human health greatly, made laws and progressively abandoned the SnPb solder in countries in the world.Therefore, the substitute of seeking the SnPb eutectic solder has become the vital task of current electron trade.Up to now, countries in the world have been developed a series of lead-free brazing in succession, and these solders mainly are based on Sn-Ag, Sn-Cu, and Sn-Ag-Cu, Sn-Zn, Sn-Bi eutectic system develops.Yet even if the Sn-Ag-Cu eutectic or the nearly eutectic solder of the tool prospect of generally acknowledging, their a lot of character all are difficult to compare with the SnPb eutectic solder.
The significant difference of Sn-Ag, Sn-Cu and Sn-Ag-Cu (SnTM, TM=Ag and/or Cu) eutectic or hypoeutectic solder and SnPb eutectic solder shows the suitable height of the former Sn content, reaches more than the 95wt%.With present modal Cu coating brazing process in, unavoidably can form intermetallic compound.The fusing point of SnTM eutectic solder is about about 220 ℃, and the operating temperature of solder joint or joint is generally at 100 ℃, even higher.Therefore, in the solid-state stage, the atom generation counterdiffusion in solder and the Cu coating, a large amount of atoms is assembled in reaction interface, reaction, makes interface compound continue growth.
Find through literature search prior art, as document " Effect of Interfacial Reaction on the TensileStrength of Sn-3.5Ag/Ni-P and Sn-37Pb/Ni-P Solder Joints " (Chen Z et al, Journal ofElectronic Materials, Vol.36,2007,17-25) result of study shows, the mechanical property of solder connector is with ageing time, the growth of compound just significantly worsens, simultaneously, fracture position is transferred to the compound interface by solder inside.Than SnPb, the mis-behave of SnTM solder connector is more obvious.And for example Chinese patent CN1603056 provides a kind of Sn-Cu-Ge lead-free brazing, CN1613597 provides a kind of Sn-Ag-Ge lead-free brazing, and more than invention has positive effect to improving the solder antioxygenic property, yet, because it is it is less to add constituent content, less to the influence of soldered fitting interfacial reaction.Chinese patent CN1962157A provides a kind of adaptive Sn-Ag-Zn lead-free brazing, but preparation technology is comparatively complicated.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of Sn-Ag-Cu-Zn-Ge lead-free brazing that suppresses solid-state interfacial reaction and preparation method thereof is provided.By forming diffusion impervious layer in reaction interface, or form tiny compound pinning at crystal boundary, the diffusion of restriction Cu atom, thus play the purpose of compound growth between the inhibitory reaction interface metal.Solved in the prior art solder and reacted with substrate metal easily, caused substrate to dissolve in a large number, formed a large amount of intermetallic compounds at the interface simultaneously, had a strong impact on the shortcoming of interface reliability, it is simple to prepare lead-free brazing technology of the present invention, easy outputization.
The present invention is achieved by the following technical solutions:
The present invention relates to suppress the Sn-Ag-Cu-Zn-Ge lead-free brazing of solid-state interfacial reaction, its component and mass percent thereof are:
Ag is 0%-3.5%;
Cu is 0%-0.7%
Zn is 0%-2%;
Ge is 0%-0.3%
Surplus is Sn.
Described Ag and Cu content only can one is 0, and the content of Zn and Ge also only can one is 0.
The present invention relates to preparation method, comprise that step is as follows as the Sn-Ag-Cu-Zn-Ge lead-free brazing of the above-mentioned solid-state interfacial reaction of inhibition:
At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and/or Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution;
Then, in alloy solution, add trace Zn foil and/or Ge grain, be incubated 2 hours, and fully stir;
Afterwards, be cooled to 300 ℃, pour in the plumbous pricker mould.
The present invention can play the molten effect of falling by add the trace Zn element in the SnTM solder alloy after, simultaneously, what is more important, the Zn element can form the Cu-Zn intermetallic compounds layer at Cu/Cu6Sn5 or Cu6Sn5/ solder interface.Cu is the essential element of interfacial reaction, and the diffusion coefficient of Cu atom in the Cu-Zn compound than Cu6Sn5 in low 2 orders of magnitude.Therefore, the continuous Cu-Zn compound layer that reaction interface forms can serve as the diffusion impervious layer of Cu atom, slows down the diffusion of Cu to Cu6Sn5/ solder interface, thereby suppresses the growth of compound layer, improves the reliability of reaction interface.Ge then is the congeners of Sn, plays an important role at raising solder wetting aspect of performance.In addition, Ge and Cu also can form intermetallic compound, and with Sn and the only limited solid solution of Ag.Therefore, when the content of Ge was enough, interface or compound layer crystal boundary can form tiny Cu-Ge compound, and pinning effect is played in the diffusion of Cu.Thereby also can suppress the growth of compound layer; In addition, Zn and Ge can both significantly improve the antioxygenic property of solder.
The present invention makes solder keep original good wettability by add a spot of Zn and Ge element in the SnTM solder alloy, in the time of advantages such as high mechanical properties, high ductibility, the fusing point of solder is had slightly reduction.Simultaneously,, and can effectively suppress the growth of solder/Cu interfacial reaction thing, improve the reliability of welding point the erodible reduction of Cu pad.
The present invention and traditional SnTM solder/Cu joint reaction interface experience 150 ℃ of heat ageing afterreaction layer thickness contrasts in 20 days no matter be simultaneously, are still added Zn and Ge separately, all help suppressing the solid-state reaction at SnTM/Cu interface.The present invention can suppress the interface compound layer in the growth of ageing step, therefore, is particularly suitable for the interconnection of high-temperature electronic components and parts, increases the reliability of solder joint.
The specific embodiment
Below embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 0.2%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-0.2Zn-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 2
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 1%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-1.0Zn-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 3
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 2%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-2.0Zn-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 4
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 1%, and Ge 0.05%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-1.0Zn-0.05Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 5
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 1%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-1.0Zn-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 6
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, and Zn 1%, and Ge 0.3%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-TM solution; Then, in alloy solution, add trace Zn foil and Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-Cu-1.0Zn-0.3Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 7
Each component and mass percent are in the present embodiment: Ag 3.5%, and Zn 1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires, be incubated 2-4 hour, fully stir, obtain uniform Sn-Ag solution; Then, in alloy solution, add trace Zn foil, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-1.0Zn/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 8
Each component and mass percent are in the present embodiment: Ag 3.5%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires, be incubated 2-4 hour, fully stir, obtain uniform Sn-Ag solution; Then, in alloy solution, add micro-Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Ag-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 9
Each component and mass percent are in the present embodiment: Cu 0.7%, and Ge 0.1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-Cu solution; Then, in alloy solution, add micro-Ge grain, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Cu-0.1Ge/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
Embodiment 10
Each component and mass percent are in the present embodiment: Cu 0.7%, and Zn 1%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-Cu solution; Then, in alloy solution, add trace Zn foil, be incubated 2 hours, and fully stir.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-Cu-1.0Zn/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
The comparative example 1
Each component and mass percent are in the present embodiment: Cu 0.7%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-Cu solution.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-0.7Cu/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
The comparative example 2
Each component and mass percent are in the present embodiment: Ag 3.5%, the Sn surplus.At first, the Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires, be incubated 2-4 hour, fully stir, obtain uniform Sn-Ag solution.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-3.5Ag/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
The comparative example 3
Each component and mass percent are in the present embodiment: Ag 3.5%, and Cu 0.7%, the Sn surplus.The Sn grain is put into 400 ℃ KCl+LiCl eutectic protection salt melt, and be warming up to 600 ℃, add high-purity Ag wires and Cu silk, be incubated 2-4 hour, fully stir, obtain uniform Sn-Ag-Cu solution.Afterwards, be cooled to 300 ℃, pour in the stainless steel mould.
Melted solder is got 100mg, is prepared into the Sn-3.5Ag-0.7Cu/Cu soldered fitting, carries out degradation.Scanning electron microscopic observation interface heterogeneous microstructure develops, and analytical reactions interface compound layer thickness.Compound layer thickness sees Table 1.
The thickness of 20 days interface compounds of 150 ℃ of heat ageings of table 1
Claims (9)
1. Sn-Ag-Cu-Zn-Ge lead-free brazing that suppresses solid-state interfacial reaction, it is characterized in that its component and mass percent thereof are: Ag is 0%-3.5%, and Cu is 0%-0.7%, and Zn is 0%-2%, and Ge is 0%-0.3%, surplus is Sn.
2. the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 1 is characterized in that, described Ag and Cu content only one be 0.
3. the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 1 is characterized in that, the content of described Zn and Ge only one be 0.
4. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 1 is characterized in that, comprises that step is as follows:
At first, the Sn grain is put into KCl+LiCl eutectic protection salt melt, heat up, add high-purity Ag wires and/or Cu silk, insulation is for the first time fully stirred, and obtains uniform Sn-TM solution;
Then, in alloy solution, add trace Zn foil and/or Ge grain, insulation for the second time, and fully stir;
Afterwards, cooling pours in the solder mould.
5. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 4 is characterized in that, described KCl+LiCl eutectic protection salt melt, and its temperature is 400 ℃.
6. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 4 is characterized in that, described intensification is to 600 ℃.
7. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 4 is characterized in that, the described insulation first time was for 2-4 hour.
8. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 4 is characterized in that, the described insulation second time is 2 hours.
9. the preparation method of the Sn-Ag-Cu-Zn-Ge lead-free brazing of the solid-state interfacial reaction of inhibition as claimed in claim 4 is characterized in that, described cooling is to 300 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102601542A (en) * | 2012-03-28 | 2012-07-25 | 华南理工大学 | Brass brazing alloy |
| CN103273217A (en) * | 2013-05-29 | 2013-09-04 | 哈尔滨工业大学深圳研究生院 | Partially-reinforced high-reliability brazing filler metal and preparing method thereof |
| RU2541249C2 (en) * | 2013-02-20 | 2015-02-10 | Открытое акционерное общество "АВТОВАЗ" | Method of making tin-based solder |
| CN105665956A (en) * | 2016-03-23 | 2016-06-15 | 徐宏达 | Soft solder alloy used for brazing aluminum and brazing aluminum alloy |
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| CN1613597A (en) * | 2003-11-07 | 2005-05-11 | 中国科学院金属研究所 | Tin and silver co-crystal solder without lead against oxidation |
| CN1905985A (en) * | 2004-07-29 | 2007-01-31 | 千住金属工业株式会社 | Lead-free solder alloy |
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| JP2002185130A (en) * | 2000-12-11 | 2002-06-28 | Fujitsu Ltd | Electronic circuit device and electronic part |
| JP2003326386A (en) * | 2002-05-13 | 2003-11-18 | Matsushita Electric Ind Co Ltd | Leadless solder alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102601542A (en) * | 2012-03-28 | 2012-07-25 | 华南理工大学 | Brass brazing alloy |
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| RU2541249C2 (en) * | 2013-02-20 | 2015-02-10 | Открытое акционерное общество "АВТОВАЗ" | Method of making tin-based solder |
| CN103273217A (en) * | 2013-05-29 | 2013-09-04 | 哈尔滨工业大学深圳研究生院 | Partially-reinforced high-reliability brazing filler metal and preparing method thereof |
| CN103273217B (en) * | 2013-05-29 | 2016-01-13 | 哈尔滨工业大学深圳研究生院 | High reliability solder of a kind of local strengthening and preparation method thereof |
| CN105665956A (en) * | 2016-03-23 | 2016-06-15 | 徐宏达 | Soft solder alloy used for brazing aluminum and brazing aluminum alloy |
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Application publication date: 20100804 |