CN101323061B - Magnesium boride granule enhancement type tin-silver-zinc compound solder and manufacture method thereof - Google Patents
Magnesium boride granule enhancement type tin-silver-zinc compound solder and manufacture method thereof Download PDFInfo
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- CN101323061B CN101323061B CN2008101071282A CN200810107128A CN101323061B CN 101323061 B CN101323061 B CN 101323061B CN 2008101071282 A CN2008101071282 A CN 2008101071282A CN 200810107128 A CN200810107128 A CN 200810107128A CN 101323061 B CN101323061 B CN 101323061B
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Abstract
The invention relates to a magnesium diboride particle reinforced type tin, silver and zinc composite solder and the preparation method. The magnesium diboride particle reinforced type tin, silver and zinc composite solder comprises a tin, silver and zinc solder and the magnesium diboride particles with 0.01-1 percent of the weight of the tin, silver and zinc solder; according to parts by weight, the tin, silver and zinc solder comprises 80-98 portions of tin, 0.1-5 portions of silver and 0.1-5 portions of zinc. The tin, silver and zinc solder, due to the addition of magnesium diboride, has better mechanical property, and can serve better under the working conditions of a thermal shock environment, with long service life. The preparation method of the solder of the invention is that, at first, button-shaped tin, silver and zinc solder is prepared; then under vacuum protection, magnesium diboride particles and button-shaped tin, silver and zinc solder are heated to 230-280 DEG C; after even stirring and cooling, the solder can be acquired, and the method is simple.
Description
Technical field
The invention belongs to lead-free solder technical field, particularly a kind of enhancement type tin-silver US zinc compound solder and preparation method thereof.
Background technology
Current, the research of novel lead-free scolder has become one of important and advanced subject of material science, and exploitation lead-free solder product is environmental protection requirement, is the main trend of development of world economy.
Solder joint is as the structure that plays connection, conduction and conductive force on the circuit board, bearing the different most of shear stresses that produce of electronic device with the baseplate material thermal coefficient of expansion, when electronic equipment moves repeatedly, be in the alternating action that solder joint in the thermal cycle will be subjected to shearing force, cause the solder joint cracking, cause electronic system to break down, therefore, require scolder to have the particularly needs satisfy to use such as mechanical property, thermal fatigue property of superior combination property.
Adopt composite methods to add to strengthen particle in existing ripe scolder is the direction that many researchers make great efforts with the performance that improves scolder always.Adding mass ratio as the researcher of U.S. Akron university in tin-lead solder is that 1～2% TiOx nano particle generates composite solder and makes the microhardness of scolder improve 50%, but, can not satisfy environmental protection requirement because this scolder remains based on solder containing pb.
Chinese invention patent 200510013430.8 has been put down in writing a kind of Zirconium oxide nano grain reinforced composite Sn-Ag welding material, mainly be to be that 96.5: 3.5 purity is in the eutectic lead-free solder of 99.99% tin and silver at mass ratio, the particle diameter of adding 1～2% is the zirconia particles of 20～30 nanometers, the remarkable refinement lead-free solder of adding energy of Zirconium oxide nano grain is at the tissue of as cast condition, microhardness has improved 15～30%, and can suppress the growth of compound between bulk metal.Therefore, utilize the characteristics that particle can improve the performance of solder alloy that strengthen, the scolder that active development has superior mechanical property and thermal fatigue property becomes the important content that current scolder is studied.
Summary of the invention
Technical problem to be solved by this invention provides a kind of magnesium boride granule enhancement type tin-silver-zinc compound solder, and this composite solder mechanical property and thermal fatigue property are superior, and the solder joint service life is long, and preparation is simple.
For solving above technical problem, the present invention takes following technical scheme:
A kind of magnesium boride granule enhancement type tin-silver-zinc compound solder, it comprises that tin silver spelter solder and quality are 0.01～1% magnesium boride granule of tin silver spelter solder, by weight, described tin silver spelter solder comprises 80～98 parts in tin, 0.1～5 part of silver, 0.1～5 part on zinc.
Preferably, described magnesium boride granule enhancement type tin-silver-zinc compound solder comprises that tin silver spelter solder and quality are 0.1～1% magnesium boride granule of tin silver spelter solder.
The particle diameter of magnesium boride granule is preferably 0.05～10 μ m.
For improving solder wettability, described tin silver spelter solder also comprises bismuth or the indium below 4 parts below 5 parts.
Be refinement scolder tissue, described tin silver spelter solder also comprises the rare earth element below 5 parts.
For improving the non-oxidizability of scolder, described tin silver spelter solder also comprises gallium or the phosphorus below 3 parts below 2.5 parts.
The present invention also will provide a kind of preparation method of above-mentioned magnesium boride granule enhancement type tin-silver-zinc compound solder, and this preparation method in turn includes the following steps:
1., tin, silver, zinc are heated to fusing by prescription in the vacuum melting furnace under the inert gas shielding, stir simultaneously, after treating that alloy mixes, water-cooled is solidified, and repeats heat fused, stirring and water-cooled coagulation step until the button-type tin silver spelter solder that obtains diameter 3.0～3.5cm;
2., by prescription with magnesium boride granule with by 1. gained tin silver spelter solder, under vacuum protection, be heated to 230～280 ℃, after stirring, cool off described magnesium boride granule enhancement type tin-silver-zinc compound solder.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
Scolder of the present invention is a matrix with tin silver spelter solder, to wherein adding the magnesium boride granule that good wetability is arranged with tin silver spelter solder matrix is arranged, magnesium diboride is good superconductor at low temperatures, at room temperature electric conductivity is similar to copper, the adding of magnesium boride granule makes tin silver spelter solder have better mechanical property, can be on active service under thermal shock environmental work condition better, service life is long.In addition, scolder preparation method of the present invention is simple.
Description of drawings
Fig. 1 is 0.1%MgB
2Strengthen the metallographic microstructure of Sn-3.5%Ag-0.9%Zn;
Fig. 2 is 0.5%MgB
2Strengthen the metallographic microstructure of Sn-3.5%Ag-0.9%Zn-1%In;
Fig. 3 is 1%MgB
2Strengthen the metallographic microstructure of Sn-3.5%Ag-0.9%Zn-1%Ga;
Fig. 4 is different content MgB
2Strengthen the Sn-3.5%Ag-0.9%Zn micro-hardness measurements;
Fig. 5 is different content MgB
2Strengthen the Sn-3.5%Ag-0.9%Zn-1%In micro-hardness measurements;
Fig. 6 is different content MgB
2Strengthen the Sn-3.5%Ag-0.9%Zn-1%Ga micro-hardness measurements.
The specific embodiment
Embodiment 1
The magnesium boride granule that comprises tin silver spelter solder and 0.1% according to the magnesium boride granule enhancement type tin-silver-zinc compound solder of present embodiment.The magnesium boride granule mean size is 8 μ m, and in the tin silver spelter solder, the mass ratio of tin, silver, zinc is 95.6: 3.5: 0.9.
The scolder that this is routine is designated as: 0.1%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn, its preparation process is as follows:
1., be that 99.99% tin, silver, zinc are heated to 1200 ℃ of fusings by recipe ratio with purity in the vacuum melting furnace under the argon shield, simultaneously in addition magnetic stirs, so that alloying component is even, water-cooled is solidified then, to reheat 1200 ℃ of fusings after the alloy upset again, simultaneously in addition magnetic stirs and water-cooled, and at least five times so repeatedly, obtaining diameter is the tin silver spelter solder buttony of 3.0～3.5cm;
2., by prescription with magnesium boride granule with the crucible of putting into by 1. gained tin silver spelter solder under the vacuum protection, be heated to 280 ℃ and stir after, water-cooled gets described 0.1%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn, its metallographic microstructure is seen Fig. 1.
Embodiment 2
The magnesium boride granule that comprises tin silver spelter solder and 0.5% according to the magnesium boride granule enhancement type tin-silver-zinc compound solder of present embodiment.The magnesium boride granule mean size is 8 μ m.Tin silver spelter solder is 94.6: 3.5: 0.9 by tin, silver, zinc, indium by mass ratio: 1 forms.
The scolder that this is routine is labeled as: 0.5%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn-1%In, its preparation process is as follows:
1., be that 99.99% tin, silver, zinc, indium are heated to 1200 ℃ of fusings by recipe ratio with purity in the vacuum melting furnace under the argon shield, simultaneously in addition magnetic stirs, so that alloying component is even, water-cooled is solidified then, to reheat 1200 ℃ of fusings after the alloy upset again, simultaneously in addition magnetic stirs and water-cooled, so repeatedly at least five times diameter is the silver-colored spelter solder of tin buttony of 3.0～3.5cm;
2., by prescription with magnesium boride granule with the crucible of putting into by 1. gained tin silver spelter solder under the vacuum protection, be heated to 270 ℃ and stir after, water-cooled gets described 0.5%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn-1%In, its metallographic microstructure is seen Fig. 2.
Embodiment 3
The magnesium boride granule that comprises tin silver spelter solder and 1% according to the magnesium boride granule enhancement type tin-silver-zinc compound solder of present embodiment.The magnesium boride granule mean size is 8 μ m.Tin silver spelter solder is that 99.99% tin, silver, zinc, gallium are 94.6: 3.5: 0.9 by mass ratio by purity: 1 forms.
The scolder that this is routine is labeled as: 1%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn-1%Ga, its preparation process is as follows:
1., be that 99.99% tin, silver, zinc, gallium are heated to 1200 ℃ of fusings by recipe ratio with purity in the vacuum melting furnace under the argon shield, simultaneously in addition magnetic stirs, so that alloying component is even, water-cooled is solidified then, to reheat 1200 ℃ of fusings after the alloy upset again, simultaneously in addition magnetic stirs and water-cooled, so repeatedly at least five times diameter is the silver-colored spelter solder of tin buttony of 3.0～3.5cm;
2., by prescription with magnesium boride granule with the crucible of putting into by 1. gained tin silver spelter solder under the vacuum protection, be heated to 260 ℃ and stir after, water-cooled gets described 1%MgB
2Strengthen Sn-3.5%Ag-0.9%Zn-1%Ga, its metallographic microstructure is seen Fig. 3.
Adopt the vickers microhardness method of testing that the enhancement mode composite solder of above-mentioned three embodiment has been carried out Mechanics Performance Testing, in the test process, load is 10g, load time is 5s, do 10 tests for each sample in experiment, the arithmetic mean of instantaneous value of test data is as sample vickers microhardness value.Test result is seen Fig. 4～Fig. 6.
By Fig. 4～6 as seen, along with MgB
2The raising of content, the microhardness of scolder raises gradually, at MgB
2The addition of particle is in 0.01～1 scope, along with MgB
2Increasing of content, the scolder mechanical property strengthens.
Claims (6)
1. magnesium boride granule enhancement type tin-silver-zinc compound solder, it is characterized in that: it comprises that tin silver spelter solder and quality are 0.1～1% magnesium boride granule of tin silver spelter solder, by weight, described tin silver spelter solder comprises 80～98 parts in tin, 0.1～5 part of silver, 0.1～5 part on zinc.
2. magnesium boride granule enhancement type tin-silver-zinc compound solder according to claim 1 is characterized in that: the particle diameter of described magnesium boride granule is 0.05～10 μ m.
3. magnesium boride granule enhancement type tin-silver-zinc compound solder according to claim 1 is characterized in that: described tin silver spelter solder also comprises bismuth or the indium below 4 parts below 5 parts.
4. magnesium boride granule enhancement type tin-silver-zinc compound solder according to claim 1 is characterized in that: described tin silver spelter solder also comprises the rare earth element below 5 parts.
5. magnesium boride granule enhancement type tin-silver-zinc compound solder according to claim 1 is characterized in that: described tin silver spelter solder also comprises gallium or the phosphorus below 3 parts below 2.5 parts.
6. the preparation method of a magnesium boride granule enhancement type tin-silver-zinc compound solder as claimed in claim 1, it is characterized in that: this preparation method in turn includes the following steps:
1., tin, silver, zinc are heated to fusing by prescription in the vacuum melting furnace under the inert gas shielding, stir simultaneously, after treating that alloy mixes, water-cooled is solidified, and repeats heat fused, stirring and water-cooled coagulation step until the button-type tin silver spelter solder that obtains diameter 3.0～3.5cm;
2., by prescription with magnesium boride granule with by 1. gained button-type tin silver spelter solder, under vacuum protection, be heated to 230～280 ℃, after stirring, cool off described magnesium boride granule enhancement type tin-silver-zinc compound solder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101071282A CN101323061B (en) | 2008-07-16 | 2008-07-16 | Magnesium boride granule enhancement type tin-silver-zinc compound solder and manufacture method thereof |
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| CN2008101071282A CN101323061B (en) | 2008-07-16 | 2008-07-16 | Magnesium boride granule enhancement type tin-silver-zinc compound solder and manufacture method thereof |
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| CN101323061B true CN101323061B (en) | 2010-06-02 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5066544A (en) * | 1990-08-27 | 1991-11-19 | U.S. Philips Corporation | Dispersion strengthened lead-tin alloy solder |
| CN1544198A (en) * | 2003-11-28 | 2004-11-10 | 北京工业大学 | Grain reinforced SnCu base composite solder ointment and preparation method thereof |
| CN1931509A (en) * | 2006-10-13 | 2007-03-21 | 华南理工大学 | Copper powder reinforced composite Sn-Zn brazing alloy and its prepn process |
-
2008
- 2008-07-16 CN CN2008101071282A patent/CN101323061B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5066544A (en) * | 1990-08-27 | 1991-11-19 | U.S. Philips Corporation | Dispersion strengthened lead-tin alloy solder |
| CN1544198A (en) * | 2003-11-28 | 2004-11-10 | 北京工业大学 | Grain reinforced SnCu base composite solder ointment and preparation method thereof |
| CN1931509A (en) * | 2006-10-13 | 2007-03-21 | 华南理工大学 | Copper powder reinforced composite Sn-Zn brazing alloy and its prepn process |
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| CN101323061A (en) | 2008-12-17 |
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