CN109926750B - Low-temperature lead-free solder alloy and vacuum casting method thereof - Google Patents
Low-temperature lead-free solder alloy and vacuum casting method thereof Download PDFInfo
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Abstract
The invention discloses a low-temperature lead-free solder alloy, which is characterized in that: the composition comprises, by mass, 8-15% of Zn, 5-12% of Bi, 4-10% of In, 0.1-1.5% of Ag, 0.05-1% of Mg, 0.01-2% of M, and the balance of Sn and inevitable impurities, wherein the mass percent of Sn is not less than 58.5%, and M is RE or at least one element of V, Zr, Ga and Ge; the tin-based low-temperature alloy solder provided by the invention has excellent wetting property and good mechanical property, the reliability of a welding spot is improved, and meanwhile, the tin-based low-temperature alloy solder is smelted under a vacuum condition, so that the influence of oxidation burning loss and oxidizing slag on the reliability of the welding spot in the smelting process of metal can be avoided, the tin-based low-temperature alloy solder can be applied to the welding of electronic components with low heating temperature, and the requirement of light and thin development of electronic products is met.
Description
Technical Field
The invention relates to a high-reliability lead-free solder alloy and a vacuum casting preparation method thereof, belonging to the field of electronic product connecting materials.
Background
With the continuous development and innovation of electronic manufacturing technology, electronic products are developing to be thinner and smaller. Due to the short and small substrate, the solder joint spacing is narrower and narrower, the requirements for the electronic packaging technology are gradually improved, the reliability of the solder joint is very important, and people pay more attention to the high-performance electronic packaging technology. In the process of manufacturing electronic products, the method for connecting components and substrates is brazing, and the quality of brazing directly influences the quality of welding, and is an important link. However, lead and its compounds are toxic and can damage the environment and human health, so that various countries have laws and regulations to limit the use of lead, and the development of lead-free electronic products is promoted.
Although Sn-Zn-based lead-free solders have been developed and produced by a number of companies in japan, Sn-Zn-based lead-free solders are rarely used in other countries because Sn-Zn-based lead-free solders are very easily oxidized due to the reactivity of Zn, which not only deteriorate wettability but also cause reduction in soldering reliability, and are difficult to preserve after being made into a solder paste, so that further efforts are required for development and popularization of Sn-Zn-based lead-free solders, and development of a low-temperature solder with low cost and high reliability is an urgent problem in the art.
Disclosure of Invention
Aiming at the defects In the prior art, the invention provides a high-reliability lead-free solder alloy which comprises, by mass, 8-15% of Zn, 5-12% of Bi, 4-10% of In, 0.1-1.5% of Ag, 0.05-1% of Mg, 0.01-2% of M, and the balance of Sn and inevitable impurities, wherein the mass percent of Sn is not less than 58.5%, and M is RE or at least one element of V, Zr, Ga and Ge.
The RE is at least one of Gd, La, Y and Ce.
The mass percent of V is 0-0.5%, the mass percent of Zr is 0-0.5%, the mass percent of Ga is 0-0.5%, and the mass percent of Ge is 0-0.5% based on the total composition of the lead-free solder alloy.
The invention also aims to provide a vacuum casting method of the low-temperature lead-free solder alloy, which comprises the following specific steps:
(1) removing oxide layers from Sn, Zn, Bi, In, Ag, Mg and M, drying and preheating to 40 ℃;
(2) under the vacuum condition, melting a part of Sn into a molten pool at 240-250 ℃, and then adding the rest Sn;
(3) after the Sn is completely melted, heating to 270 ℃, adding Bi, In, Ag and M into the melted Sn for 2-4 times respectively, keeping the temperature at 250-270 ℃ during the process, and preserving the heat at 270 ℃ for 5-10 minutes after all the alloys are added; then adding Zn and Mg, stirring and uniformly mixing at 260-270 ℃, standing for 10-20 minutes after stirring, and skimming surface scum at 270 ℃ to obtain a tin alloy melt; and carrying out vacuum casting on the tin alloy melt at 270 ℃ to obtain a lead-free solder tin alloy casting.
And in the step (2), the Sn melted first accounts for 20-40% of the total mass of the Sn.
The vacuum casting is to pour a tin alloy melt into a metal mold preheated to 100-120 ℃ at 270 ℃, and cool and mold in vacuum.
The invention mainly improves the problems of poor wettability of the solder containing the zinc-tin-based alloy and the like by improving the surface tension of the solder melt and improving the oxidability, the addition of the alloy element Bi reduces the surface tension of the solder containing the zinc-tin-based alloy, meanwhile, the addition of the alloy element In and trace rare earth elements can also improve the wettability of the solder alloy, the addition of the Mg element strengthens the mechanical property of the alloy, In addition, the addition of the elements such as V, Zr and the like and the alloy form intermetallic compounds, and simultaneously, the formation of coarse Sn-Zn eutectic phase is inhibited, and the effect of refining grains is achieved; the vacuum casting process can avoid burning loss of metals such as Zn, Mg and the like, simultaneously does not need huge processing equipment, can pour and form parts with complex shapes, saves metals, reduces the cost, reduces the working hours and the like, improves the market competitiveness of the novel solder alloy, and is suitable for being popularized to large-scale industrial production.
Compared with the prior art, the invention has the following beneficial effects:
1. the alloy raw materials are all pure metals, the sources are wide, the infiltration of harmful impurity elements can be effectively prevented, no impurity elements infiltrate in the whole preparation process, and the impurity content of the prepared low-temperature lead-free solder alloy is extremely low;
2. the vacuum casting process can effectively avoid the burning loss and oxidation phenomena of metals such as Zn, Mg and the like, can remove easily oxidized impurity components in the alloy, and effectively improves the mechanical property of the low-temperature lead-free solder alloy;
3. RE is an effective element for improving the wettability of the solder, and the elements can improve the oxidation resistance of the solder; meanwhile, rare earth and Sn element in the alloy form rare earth compound, so that the mechanical property of the alloy can be obviously improved;
4. the alloy material prepared by the method has the characteristics of high tensile strength, high yield strength, high elongation, good wettability, good oxidation resistance and the like, and meanwhile, the welded welding spot has uniform microstructure, good thermal fatigue and creep property and low cost, can be applied to welding of electronic components with low heating temperature, and meets the requirements of lightening and thinning development of electronic products.
Drawings
FIG. 1 is an as-cast SEM image of the low temperature solder alloy prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1: the high-reliability low-temperature lead-free solder alloy comprises the following components in percentage by mass: 11% of Zn, 8.5% of Bi, 7% of In, 0.8% of Ag, 0.5% of Mg, 0.3% of V, 0.3% of Zr, 0.3% of Ga, 0.3% of Ge, and the balance of Sn and inevitable impurities.
The preparation method comprises (1) respectively polishing industrial pure tin (Sn: 99.95 wt%), industrial pure bismuth (Bi: 99.95 wt%), industrial pure zinc (Zn: 99.9 wt%) and indium, silver, magnesium, vanadium, zirconium, gallium and germanium with 320 mesh sand paper to remove oxide layer, respectively placing into a blast drying oven (40 deg.C) for drying and preheating; (2) carrying out alloy casting by using a graphite crucible, cleaning the surfaces of the crucible, a slag removing tool, a bell jar and the like before use to remove impurities, then placing the crucible, the slag removing tool, the bell jar and the like in a 40 ℃ oven to bake and remove water before use, heating the temperature gradient of a vacuum smelting furnace to 250 ℃, melting pure tin accounting for 30 percent of the total mass of the pure tin into a molten pool at 245 ℃, and then adding the residual pure tin; after the pure tin is completely melted, heating to 270 ℃; (3) sequentially adding indium, bismuth, silver, vanadium, zirconium, gallium and germanium metals for 3 times respectively, keeping the temperature constant at 265 ℃, and preserving the heat for 7 minutes at 270 ℃ after all the metals are added; (4) after all alloy elements are melted, keeping the temperature of the melt at 270 ℃, adding industrial pure zinc and magnesium metals, pressing the metals into the tin alloy melt by using a bell jar during adding, and stirring to fully melt the metals; (5) stirring at 265 ℃ after all alloy components are completely melted, standing for 15 minutes after stirring, and skimming surface scum at 270 ℃ to obtain a tin alloy melt; (6) and carrying out gravity casting on the tin alloy melt at 270 ℃, wherein the casting process is to cast the tin alloy melt into a metal mold preheated to 110 ℃ at 270 ℃, and cooling and forming in vacuum to obtain a tin alloy casting.
The solidus temperature of the low-temperature solder alloy in this example was 174.8 ℃, the as-cast room-temperature tensile strength was 103.2MPa, the elongation was 44%, and the post-weld shear strength was 42.5MPa, and further, the maximum wetting force in the solderability test of the solder alloy in this example was 0.7531 mN.
The high-reliability lead-free solder alloy material prepared in the embodiment has accurate components and no distinguishable cracks, and microstructure analysis shows that the alloy has no air holes and obvious defects, as shown in figure 1, so that the tin alloy material prepared by the method has uniform tissue distribution, no oxidation inclusion and component segregation phenomena, good wettability and mechanical properties, and welded welding spots have uniform microstructure, good thermal fatigue and creep property, and high reliability requirements.
Example 2: the high-reliability lead-free solder alloy comprises the following components in percentage by mass: 8% of Zn, 5% of Bi, 4% of In, 0.1% of Ag, 0.05% of Mg, 0.01% of V, and the balance of Sn and inevitable impurities.
The preparation method comprises (1) grinding industrial pure tin (Sn: 99.95 wt%), industrial pure bismuth (Bi: 99.95 wt%) and industrial pure zinc (Zn: 99.9 wt%) and indium, silver, magnesium and vanadium respectively with 320 mesh sand paper to remove oxide layer, and drying and preheating in a blast drying oven (40 deg.C); (2) carrying out alloy casting by using a graphite crucible, cleaning the surfaces of the crucible, a slag removing tool, a bell jar and the like before use to remove impurities, then placing the crucible, the slag removing tool, the bell jar and the like in a 40 ℃ oven to bake and remove water before use, heating the temperature gradient of a vacuum smelting furnace to 250 ℃, melting pure tin accounting for 20 percent of the total mass of the pure tin into a molten pool at 240 ℃, and then adding the residual pure tin; after the pure tin is completely melted, heating to 270 ℃; (3) sequentially adding indium, bismuth, silver and vanadium for 2 times, keeping the temperature constant at 250 ℃, and preserving the heat at 270 ℃ for 5 minutes after all the metals are added; (4) after all alloy elements are melted, keeping the temperature of the melt at 270 ℃, adding industrial pure zinc and magnesium metals, pressing the metals into the tin alloy melt by using a bell jar during adding, and stirring to fully melt the metals; (5) stirring at 260 ℃ after all the alloy components are completely melted, standing for 10 minutes after stirring, and skimming the surface scum at 270 ℃ to obtain a tin alloy melt; (6) and carrying out gravity casting on the tin alloy melt at 270 ℃, wherein the casting process is to cast the tin alloy melt into a metal mold preheated to 100 ℃ at 250 ℃, and cooling and forming in vacuum to obtain a tin alloy casting.
The solidus temperature of the low-temperature solder alloy in this example was 178.5 ℃, the as-cast room-temperature tensile strength was 90.5MPa, the elongation was 35%, the shear strength of the solder joint after soldering was 37.9MPa, and further, the maximum wetting force in the solderability test of the solder alloy in this example was 0.6850 mN.
The high-reliability lead-free solder alloy material finally prepared in the invention has accurate components and no distinguishable cracks, and the microstructure analysis shows that the alloy has no air holes and obvious defects. Therefore, the tin alloy material obtained by the invention has uniform tissue distribution, no oxide inclusion and component segregation phenomena, good wettability and mechanical property, uniform microstructure of the welded welding spot, good thermal fatigue and creep property and high reliability requirement.
Example 3: the high-reliability lead-free solder alloy comprises the following components in percentage by mass: 15% of Zn, 12% of Bi, 10% of In, 1.5% of Ag, 1% of Mg, 0.5% of V, 0.5% of Zr, 0.5% of Ga, 0.5% of Ge and the balance of Sn and inevitable impurities.
The preparation method comprises (1) respectively polishing industrial pure tin (Sn: 99.95 wt%), industrial pure bismuth (Bi: 99.95 wt%) and industrial pure zinc (Zn: 99.9 wt%) and indium, silver, magnesium, vanadium, zirconium, gallium and germanium with 320 mesh sand paper to remove oxide layer, respectively placing into a blast drying oven (40 deg.C) for drying and preheating; (2) carrying out alloy casting by using a graphite crucible, cleaning the surfaces of the crucible, a slag removing tool, a bell jar and the like before use to remove impurities, then placing the crucible, the slag removing tool, the bell jar and the like in a 40 ℃ oven to bake and remove water before use, heating the temperature gradient of a vacuum smelting furnace to 250 ℃, melting pure tin accounting for 40 percent of the total mass of the pure tin into a molten pool at 250 ℃, and adding the residual pure tin; after the pure tin is completely melted, heating to 270 ℃; (3) sequentially adding indium, bismuth, silver, vanadium, zirconium, gallium and germanium metals for 4 times, keeping the temperature constant at 270 ℃, and preserving the temperature at 270 ℃ for 10 minutes after all the metals are added; (4) after all alloy elements are melted, keeping the temperature of the melt at 270 ℃, adding industrial pure zinc and magnesium metals, pressing the metals into the tin alloy melt by using a bell jar during adding, and stirring to fully melt the metals; (5) stirring at 270 ℃ after all the alloy components are completely melted, standing for 20 minutes after stirring, and skimming the surface scum at 270 ℃ to obtain a tin alloy melt; (6) and (2) carrying out gravity casting on the tin alloy melt at 250 ℃, wherein the casting process is to cast the tin alloy melt into a metal mold preheated to 120 ℃ at 270 ℃, and cooling and forming in vacuum to obtain a tin alloy casting.
The solidus temperature of the low-temperature solder alloy in the example is 167.5 ℃, the tensile strength at the casting room temperature is 79.9MPa, the elongation is 42%, the shear strength of the welding spot after welding is 39.9MPa, and in addition, the maximum wetting force in the solderability test of the solder alloy in the example is 0.7100 mN.
The high-reliability lead-free solder alloy material finally prepared in the invention has accurate components and no distinguishable cracks, and the microstructure analysis shows that the alloy has no air holes and obvious defects. Therefore, the tin alloy material obtained by the invention has uniform tissue distribution, no oxide inclusion and component segregation phenomena, good wettability and mechanical property, uniform microstructure of the welded welding spot, good thermal fatigue and creep property, and high reliability requirement
Example 4: the high-reliability lead-free solder alloy comprises the following components in percentage by mass: 10% of Zn, 8% of Bi, 8% of In, 1% of Ag, 0.5% of Mg, 0.1% of Gd, 0.1% of La, and the balance of Sn and inevitable impurities.
The preparation method comprises (1) respectively polishing industrial pure tin (Sn: 99.95 wt%), industrial pure bismuth (Bi: 99.95 wt%) and industrial pure zinc (Zn: 99.9 wt%) and indium, magnesium, silver, gadolinium and lanthanum with 320 mesh sand paper to remove oxide layer, and respectively drying and preheating in a blast drying oven (40 deg.C); (2) carrying out alloy casting by using a graphite crucible, cleaning the surfaces of the crucible, a slag removing tool, a bell jar and the like before use to remove impurities, then placing the crucible, the slag removing tool, the bell jar and the like in a 40 ℃ oven to bake and remove water before use, heating the temperature gradient of a vacuum smelting furnace to 250 ℃, melting pure tin accounting for 25 percent of the total mass of the pure tin into a molten pool at 240 ℃, and then adding the residual pure tin; after the pure tin is completely melted, heating to 270 ℃; (3) sequentially adding indium, bismuth, silver, gadolinium and lanthanum for 2 times, keeping the temperature constant at 250 ℃, and preserving the heat at 270 ℃ for 5 minutes after all the metals are added; (4) after all alloy elements are melted, keeping the temperature of the melt at 270 ℃, adding industrial pure zinc and magnesium metals, pressing the metals into the tin alloy melt by using a bell jar during adding, and stirring to fully melt the metals; (5) stirring at 260 ℃ after all the alloy components are completely melted, standing for 15 minutes after stirring, and skimming the surface scum at 270 ℃ to obtain a tin alloy melt; (6) and carrying out gravity casting on the tin alloy melt at 270 ℃, wherein the casting process is to cast the tin alloy melt into a metal mold preheated to 100 ℃ at 270 ℃, and cooling and forming in vacuum to obtain a tin alloy casting.
The solidus temperature of the low-temperature solder alloy in this example was 174.2 ℃, the as-cast room-temperature tensile strength was 93.1MPa, the elongation was 37%, and the post-weld shear strength was 39.2MPa, and further, the maximum wetting force in the solderability test of the solder alloy in this example was 0.6605 mN.
The high-reliability lead-free solder alloy material finally prepared in the invention has accurate components and no distinguishable cracks, and the microstructure analysis shows that the alloy has no air holes and obvious defects. Therefore, the tin alloy material obtained by the invention has uniform tissue distribution, no oxide inclusion and component segregation phenomena, good wettability and mechanical property, uniform microstructure of the welded welding spot, good thermal fatigue and creep property and high reliability requirement.
Example 5: the high-reliability lead-free solder alloy comprises the following components in percentage by mass: 12% of Zn, 11% of Bi, 7% of In, 0.5% of Ag, 0.8% of Mg, 0.5% of Gd, 0.5% of La, 0.5% of Y, 0.5% of Ce, and the balance of Sn and inevitable impurities.
The preparation method comprises (1) respectively polishing industrial pure tin (Sn: 99.95 wt%), industrial pure bismuth (Bi: 99.95 wt%) and industrial pure zinc (Zn: 99.9 wt%) and indium, magnesium, silver, gadolinium, lanthanum, yttrium and cerium with 320 mesh sand paper to remove oxide layer, respectively placing into a blast drying oven (40 deg.C) for drying and preheating; (2) carrying out alloy casting by using a graphite crucible, cleaning the surfaces of the crucible, a slag removing tool, a bell jar and the like before use to remove impurities, then placing the crucible, the slag removing tool, the bell jar and the like in a 40 ℃ oven to bake and remove water before use, heating the temperature gradient of a vacuum smelting furnace to 250 ℃, melting pure tin accounting for 35 percent of the total mass of the pure tin into a molten pool at 250 ℃, and adding the residual pure tin; after the pure tin is completely melted, heating to 270 ℃; (3) sequentially adding indium, bismuth, silver, gadolinium, lanthanum, yttrium and cerium for 4 times, keeping the temperature constant at 270 ℃, and preserving the temperature for 10 minutes at 270 ℃ after all the metals are added; (4) after all alloy elements are melted, keeping the temperature of the melt at 270 ℃, adding industrial pure zinc and magnesium metals, pressing the metals into the tin alloy melt by using a bell jar during adding, and stirring to fully melt the metals; (5) stirring at 270 ℃ after all the alloy components are completely melted, standing for 20 minutes after stirring, and skimming the surface scum at 270 ℃ to obtain a tin alloy melt; (6) and carrying out gravity casting on the tin alloy melt at 270 ℃, wherein the casting process is to cast the tin alloy melt into a metal mold preheated to 115 ℃ at 270 ℃, and cooling and forming in vacuum to obtain a tin alloy casting.
The solidus temperature of the low-temperature solder alloy in this example was 169.5 ℃, the as-cast room-temperature tensile strength was 97.6MPa, the elongation was 36%, the post-weld shear strength was 42.3MPa, and further, the maximum wetting force in the solderability test of the solder alloy in this example was 0.7301 mN.
The high-reliability lead-free solder alloy material finally prepared in the invention has accurate components and no distinguishable cracks, and the microstructure analysis shows that the alloy has no air holes and obvious defects. Therefore, the tin alloy material obtained by the invention has uniform tissue distribution, no oxide inclusion and component segregation phenomena, good wettability and mechanical property, uniform microstructure of the welded welding spot, good thermal fatigue and creep property and high reliability requirement.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (5)
1. A low temperature lead-free solder alloy characterized by: the composition comprises, by mass, 8-15% of Zn, 5-12% of Bi, 4-10% of In, 0.1-1.5% of Ag, 0.05-1% of Mg, 0.01-2% of M, and the balance of Sn and inevitable impurities, wherein the mass percent of Sn is not less than 58.5%, and M is RE or at least one element of V, Zr, Ga and Ge;
the vacuum casting method of the low-temperature lead-free solder alloy comprises the following steps:
(1) removing oxide layers from Sn, Zn, Bi, In, Ag, Mg and M, drying and preheating to 40 ℃;
(2) under the vacuum condition, melting a part of Sn into a molten pool at 240-250 ℃, and then adding the rest Sn;
(3) after the Sn is completely melted, heating to 270 ℃, adding Bi, In, Ag and M into the melted Sn for 2-4 times respectively, keeping the temperature at 250-270 ℃ during the process, and preserving the heat at 270 ℃ for 5-10 minutes after all the alloys are added; then adding Zn and Mg, stirring and uniformly mixing at 260-270 ℃, standing for 10-20 minutes after stirring, and skimming surface scum at 270 ℃ to obtain a tin alloy melt; and carrying out vacuum casting on the tin alloy melt at 270 ℃ to obtain a lead-free solder tin alloy casting.
2. The low temperature lead-free solder alloy of claim 1, wherein: RE is at least one of Gd, La, Y and Ce.
3. The low temperature lead-free solder alloy of claim 1, wherein: the mass percent of V is 0-0.5%, the mass percent of Zr is 0-0.5%, the mass percent of Ga is 0-0.5%, and the mass percent of Ge is 0-0.5% based on the total composition of the lead-free solder alloy.
4. The low temperature lead-free solder alloy of claim 1, wherein: in the step (2), the Sn melted first accounts for 20-40% of the total mass of the Sn.
5. The low temperature lead-free solder alloy of claim 1, wherein: the vacuum casting is to pour the tin alloy melt into a metal mold preheated to 100-120 ℃ at 270 ℃, and cool and mold in vacuum.
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| CN1139607A (en) * | 1995-06-30 | 1997-01-08 | 三星电机株式会社 | Non-lead solder with fine mechanical property |
| JP4453473B2 (en) * | 2003-10-10 | 2010-04-21 | パナソニック株式会社 | Lead-free solder alloys, solder materials and solder joints using them |
| CN101612694A (en) * | 2004-04-21 | 2009-12-30 | 日本电气株式会社 | Scolding tin and use the mounted article of this scolding tin |
| CN1281372C (en) * | 2004-07-16 | 2006-10-25 | 北京工业大学 | SnZn series lead-free welding flux |
| CN101417375B (en) * | 2007-10-23 | 2010-12-29 | 北京有色金属研究总院 | Leadless welding alloy for welding electronic elements |
| CN102152022A (en) * | 2011-04-18 | 2011-08-17 | 宁波喜汉锡焊料有限公司 | Corrosion-resistant Sn-Zn-based lead-free solder with high oxidation resistance |
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