CN115647644A - Five-pack eutectic high-toughness low-temperature tin-bismuth series solder and preparation method thereof - Google Patents
Five-pack eutectic high-toughness low-temperature tin-bismuth series solder and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 16
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Abstract
The five-pack eutectic high-toughness low-temperature tin-bismuth system solder comprises the following components in percentage by mass: 0.431% of In, 0.019% of Cu, 0.602% of Sb and 56.86% of Bi, and the balance of Sn and inevitable impurities. The five-membered eutectic tin-bismuth series solder with high toughness is obtained by the aid of alloy component design assisted by thermodynamic calculation, has excellent mechanical properties, and is suitable for the field of low-temperature welding of microelectronic and photovoltaic packaging.
Description
Technical Field
The invention relates to a quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth series solder with the melting temperature close to the Sn58Bi eutectic temperature and a preparation method thereof, belonging to the technical field of materials for microelectronic interconnection and photovoltaic solder strip welding.
Background
With the gradual increase of the requirements of high-density electronic information equipment and photovoltaic modules, the rapid development of low-temperature solders for microelectronics and photovoltaics is driven. At present, sn-Ag-Cu series and Sn-Pb series alloys are commonly used in the fields of microelectronics and photovoltaics, and the problems of post-welding bending deformation and the like of a substrate are easily caused due to higher melting point and higher heat input of the Sn-Ag-Cu series alloys. In addition, increasingly strict environmental requirements at home and abroad present the trend that lead-free alloy gradually replaces Sn-Pb alloy. The tin-bismuth alloy has lower welding temperature, good wetting property, higher tensile strength and lower alloy cost. Therefore, the lead-free low-temperature tin-bismuth alloy becomes a development trend of low-temperature solder for microelectronic interconnection and photovoltaic packaging.
Tin-based solder alloys are used in the form of solder joints in the field of microelectronic interconnects and photovoltaic packaging. The reliability problem of the welding spot under the service condition and the solution of microalloying are approximately as follows: (1) When the solder joint is in the service process of thermal cycle and aging for a long time, an intermetallic compound (IMC) layer at the interface between the solder and the copper-clad plate is gradually thickened, so that the reliability of the solder joint is gradually reduced. According to a previous study (Beluakov S A, nishimura T, akaiwa T, et al. Role of Bi, sb and In microstructure formation and properties of Sn-0.7Cu-0.05Ni-X BGA interconnections [ C]//2019International Conference on Electronics Packaging (ICEP). 2019.), the addition of elements such as Ni, sb, in and the like can reduce the growth rate of IMC In the aging process, thereby inhibiting the thickening of the IMC layer and improving the reliability of welding spots; (2) In the welding process of the welding material and the substrate and the service process of the welding point, the Cu element of the substrate diffuses into the welding material through the interface, the IMC layer of the interface thickens, the reliability of the welding point is reduced, trace Cu element is usually added into the welding material alloy to reduce the diffusion of the Cu element of the substrate to the interface, the concentration gradient is reduced, and the dissolution of the Cu element of the substrate is reduced. CN 111182999A, a patent of metal industries co, mentions that a solder alloy containing Cu suppresses diffusion of Cu atoms of a substrate to an interface and an inside of a solder, thereby reducing solubility of Cu elements; (3) In addition, bi element inside the solder joint gradually segregates to the Interface, the solder joint may fail at the Interface with rich Bi phase due to the brittleness of Bi phase, and the addition of trace Ag element can inhibit Segregation of Bi element at the Interface (Zhang Q K, zou H F, zhang Z F. Ingredients of Substrate Alloying and reflection Temperature on Bi Segregation at Sn-Bi/Cu Interface [ J].Journal of Electronic Materials,2011,40(11):2320-2328.), and the reliability of the welding spot is improved. In summary, in order to obtain a solder joint with excellent reliability, the solder alloy needs to be subjected to multi-element micro-alloying treatment (CN 106216872B), wherein the alloying effect is significantly affected by the types and contents of the added elements. In the tin alloy micro-alloying process, the added alloy elements comprise Cu, ag, sb, in and the like, wherein the elements except Sb and In are dissolved In a matrix In a solid solution mode, and the rest elements mainly exist In a mode of forming IMC with the tin matrix, the mechanical property of the alloy is damaged due to excessive IMC, such as Ag addition, slight strength increase, more plasticity reduction, damage toughness (Yang T, zhao X, xiong Z, et al 3 Sn[J]Materials Science and Engineering: A,2020, 785.). Therefore, designing and preparing multiple microalloyed solders is the key to improving the reliability performance of solder joints.
In the development process of the lead-free low-temperature tin-bismuth system solder alloy, the requirement of low-temperature welding is required to be met besides multi-element micro-alloying. However, the conventional method of reducing Bi content to improve the toughness of the alloy can greatly improve the welding temperature of the alloy (Cai S, luo X, peng J, et al. Deformation mechanism of variations Sn-xBi alloys under Materials tests [ J ]. Advanced Composites and Hybrid Materials,2021, 20.), and can not match the low-temperature welding process conditions of the prior applicable eutectic alloy.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth series solder so as to enable the elongation of the solder alloy to be obviously improved compared with that of SnBi58 binary alloy under the conditions of not reducing the Bi content, not improving the melting point of the solder alloy and not reducing the tensile strength and the phase structure area fraction, thereby improving the toughness of the solder alloy and being beneficial to solving the problems of poor toughness of the SnBi58 binary alloy and insignificant improvement of the toughness of the tin-bismuth series quaternary-wrapped eutectic alloy. The invention also provides a preparation method of the five-element-wrapped eutectic high-toughness low-temperature tin-bismuth series solder.
The purpose of the invention is realized by the following technical scheme:
the five-element-coated eutectic high-toughness tin-bismuth-based solder comprises the following components in percentage by mass: 0.431% of In, 0.019% of Cu, 0.602% of Sb and 56.86% of Bi, and the balance of Sn and inevitable impurities.
The preparation method of the five-element-coated eutectic high-toughness tin-bismuth-series solder comprises the following steps:
1) Preparing SnCu10 intermediate alloy;
2) Obtaining the mass percentages of all components of the five-element-coated eutectic high-toughness tin-bismuth-series solder through thermodynamic calculation, adding the SnCu10 intermediate alloy and metals Sn, bi, in and Sb according to the calculated mass percentages into a lead-free titanium-tin furnace to be melted, covering an antioxidant on the surface of the alloy, heating the alloy to 400 ℃, preserving the temperature for 30min, casting the alloy into a mold to prepare an alloy ingot, wherein the alloy undergoes the following coating eutectic reaction In the solidification process, and Liquid + SbSn = InSb + Cu 6 Sn 5 - η + (Sn) + (Bi) to obtain the five-membered eutectic high-toughness tin-bismuth-based solder, the melting temperature of which is 144.7 ℃.
Further, the preparation method of the SnCu10 intermediate alloy comprises the following steps: respectively adding Sn and Cu with the purity of 99.99wt.% into a vacuum melting furnace according to the mass ratio of 90 to 10, vacuumizing to 3 x 10-3MPa, filling nitrogen, heating to 1100 ℃ for melting, preserving heat for 30min, and then carrying out vacuum casting to prepare the SnCu10 intermediate alloy, wherein the melting point of the alloy is 450 ℃.
The welding spot or welding seam formed by the quinary-pack eutectic high-toughness lead-free tin bismuth solder is formed by general tin paste reflow soldering, tin bar wave soldering or tin material hot melting soldering, and the hot melting soldering comprises a soldering lug, a soldering strip, BGA (ball grid array), a welding wire and the like.
The invention has the following advantages:
(1) The optimized components of the five-element-clad eutectic high-toughness low-temperature tin-bismuth series solder obtained through thermodynamic calculation are verified through experiments, compared with SnBi58 and a four-element-clad eutectic alloy, the tensile strength of the solder is not obviously changed, the elongation is obviously improved, and the lifting rate exceeds 150%;
(2) The melting temperature of the high-toughness lead-free tin-bismuth solder alloy obtained by the invention is lower than 145 ℃, is close to the temperature of SnBi58 alloy, is lower than the temperature of quaternary package eutectic alloy, and can be matched with the eutectic alloy low-temperature welding process;
(3) In the five-element microalloying process, in, sb and Cu alloy elements with fixed contents are added, so that the problems of over-thick IMC layer, bi segregation, cu dissolution and the like are solved, and the later-stage welding spot reliability is improved;
(4) In the invention, the intermediate alloy SnCu10 with low melting point and easy dissolution is prepared before, and then the low melting point metal elements such as Sn, bi and the like are added. Compared with the preparation mode of separately adding high-melting-point metal simple substance Cu for multiple times, the method for preparing the five-element-wrapped eutectic high-toughness low-temperature tin-bismuth-based solder disclosed by the invention has the advantages of simple and convenient process, high metal utilization rate, uniform alloy components and the like.
Drawings
FIG. 1 is a graph of tensile properties of alloys of example 1, comparative example 1 and comparative example 2;
FIG. 2 is a DSC plot of the alloy of example 1;
FIG. 3 is a DSC plot of the alloy of comparative example 1;
FIG. 4 is a DSC plot of the alloy of comparative example 2;
FIG. 5 is a microstructure SEM mirror of the alloy of example 1;
FIG. 6 is a SEM image of the microstructure of the alloy of comparative example 1;
FIG. 7 is a SEM image of the microstructure of the alloy of comparative example 2;
FIG. 8 is a SEM image of a low tensile fracture of the alloy of example 1;
FIG. 9 is a SEM image of a low tensile fracture of the alloy of comparative example 1;
FIG. 10 is a SEM image of low tensile fracture of the alloy of comparative example 2;
FIG. 11 is a SEM image of high tensile fracture of the alloy of example 1;
FIG. 12 is a SEM image of high tensile fracture of the alloy of comparative example 1;
fig. 13 is a SEM image of high tensile fracture of the alloy of comparative example 2.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the examples.
The five-pack eutectic high-toughness tin-bismuth-based solder comprises the following components in percentage by mass: 0.431% of In, 0.019% of Cu, 0.602% of Sb and 56.86% of Bi, and the balance of Sn and inevitable impurities.
The preparation method of the five-element-coated eutectic high-toughness tin-bismuth-series solder comprises the following steps:
1) Preparing SnCu10 intermediate alloy;
2) Obtaining the mass percentages of all components of the five-element-coated eutectic high-toughness tin-bismuth-series solder through thermodynamic calculation, adding the SnCu10 intermediate alloy and metals Sn, bi, in and Sb according to the calculated mass percentages into a lead-free titanium-tin furnace to be melted, covering an antioxidant on the surface of the alloy, heating the alloy to 400 ℃, preserving the temperature for 30min, casting the alloy into a mold to prepare an alloy ingot, wherein the alloy undergoes the following coating eutectic reaction In the solidification process, and Liquid + SbSn = InSb + Cu 6 Sn 5 - η + (Sn) + (Bi) to obtain the five-membered eutectic high-toughness tin-bismuth-based solder, the melting temperature of which is 144.7 ℃.
Further, the preparation method of the SnCu10 intermediate alloy comprises the following steps: respectively adding Sn and Cu with the purity of 99.99wt.% into a vacuum melting furnace according to the mass ratio of 90 to 10, vacuumizing to 3 x 10-3MPa, filling nitrogen, heating to 1100 ℃ for melting, preserving heat for 30min, and then carrying out vacuum casting to prepare the SnCu10 intermediate alloy, wherein the melting point of the alloy is 450 ℃.
Example 1
A quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth series solder is obtained by thermodynamic calculation according to mass percentage, and comprises the following preferred components: 56.86% of Bi, 0.431% of In, 0.019% of Cu, 0.602% of Sb and the balance of Sn and inevitable impurities. The preparation method of the five-membered eutectic high-toughness low-temperature tin-bismuth series solder comprises the following steps:
(1) Adding Sn with the purity of 99.99% and Cu with the purity of 99.99% into a vacuum smelting furnace according to the alloy proportion of 90;
(2) Sn with the purity of 99.99 percent, sb with the purity of 99.99 percent, in with the purity of 99.99 percent and Bi with the purity of 99.99 percent are added into a lead-free titanium tin furnace for melting. Covering acrylic acid modified rosin on the surface of the alloy, heating the alloy to 400 ℃, preserving heat for 30min, and casting the alloy in a mold to prepare a SnBi56.86Sb0.60In0.43Cu0.02 solder alloy ingot, namely the five-membered eutectic high-toughness low-temperature tin-bismuth series solder, wherein the melting temperature of the solder is 144.7 ℃.
Comparative example 1
Preparing the SnBi58 alloy. The alloy and the preparation method are as follows: sn with the purity of 99.99 percent and Bi with the purity of 99.99 percent are respectively put into a lead-free titanium tin furnace according to the alloy proportion, and 10g of acrylic acid modified rosin is scattered on the upper layer of the metal. And heating the metal to 400 ℃, preserving heat for 30min, and casting the metal in a mould to prepare the SnBi58 alloy ingot.
Comparative example 2
Preparing a four-element package eutectic tin-bismuth system solder SnBi55.3Sb0.81Ag0.55, wherein the four-element package eutectic solder comprises the following components in percentage by mass through thermodynamic calculation: 55.30 percent of Bi, 0.81 percent of Sb, 0.55 percent of Ag, and the balance of Sn and inevitable impurities. The preparation was the same as in example 1 except that no Cu metal was added and the content of the microalloying element was changed.
Test:
(1) Respectively cutting the alloy ingots of example 1, comparative example 1 and comparative example 2 into tensile samples with the length of 16mm, the thickness of 1mm and the length of a gauge length section of 5 mm;
(2) The tensile strength and elongation of the alloy were determined on a high throughput tensile testing apparatus. Three tensile samples were tested per data point and averaged as shown in table 1, and the stress strain curve for the tensile sample was taken near the performance average as shown in fig. 1. The elongation of the SnBi56.86Sb0.60In0.43Cu0.02 five-element wrapped eutectic high-toughness low-temperature tin-bismuth series solder is higher than that of the SnBi58 binary alloy and the four-element wrapped eutectic alloy SnBi55.3Sb0.81Ag0.55. The microstructure of SnBi56.86Sb0.60In0.43Cu0.02 five-element wrapped eutectic high-toughness low-temperature tin-bismuth solder alloy, snBi58 binary alloy and four-element wrapped eutectic alloy SnBi55.3Sb0.81Ag0.55 are shown in figure 5, figure 6 and figure 7. The low-power stretching fracture necking phenomenon of the quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth-based solder alloy is obvious and is toughness fracture, while the low-power stretching fracture phenomenon of the SnBi58 binary alloy and the SnBi55.3Sb0.81Ag0.55 quaternary-wrapped eutectic alloy is not obvious and is brittle fracture, and the fracture is shown in figures 8, 9 and 10. The high tensile fracture of the five-element-wrapped eutectic high-toughness low-temperature tin-bismuth-based solder alloy has a large number of distributed dimples and deeper dimples, which indicates that the fracture mode of the alloy is ductile fracture, the high tensile fracture of the alloy in the comparative example 1 and the alloy in the comparative example 2 has no large number of dimples, and the cleavage step is partially visible, so that the fracture mode of the alloy is mainly brittle fracture mode, as shown in fig. 11, fig. 12 and fig. 13.
(3) The melting point test of the alloy is measured on a differential thermal analyzer, the heating rate is 5 ℃/min, and the sample is measured under the argon condition, and the results are shown in figures 2, 3 and 4. The melting point of the SnBi56.86Sb0.60In0.43Cu0.02 five-element wrapped eutectic high-toughness low-temperature tin-bismuth series solder is not obviously increased, and the value of the melting point is close to the melting point of the SnBi58 binary alloy and the four-element wrapped eutectic tin-bismuth series solder SnBi55.3Sb0.81Ag0.55, so that the SnBi56.86Sb0.60In0.43Cu0.02 five-element wrapped eutectic high-toughness low-temperature tin-bismuth series solder can be matched with the welding process of the SnBi58 binary alloy in the actual welding process, and the low-temperature welding requirement is met.
And (3) counting the phase area fraction:
scanning electron microscope images of alloy samples of example 1, comparative example 1 and comparative example 2 are taken for 3 pieces at the same times, the area fractions of the eutectic structure (white phase region) of comparative example 1, the tin-bismuth-coated eutectic structure (white phase region) of comparative example 2 and the beta-Sn phase (gray phase region) are counted by image J software, and the area fractions of the tin-bismuth-coated eutectic structure (white phase) and the beta-Sn phase (gray phase) of the three alloys tend to be consistent by taking an average value, as shown in Table 2. Compared with the SnBi58 binary alloy and the four-element wrapped eutectic tin-bismuth system solder SnBi55.3Sb0.81Ag0.55 and SnBi56.86Sb0.60In0.43Cu0.02 five-element wrapped eutectic high-toughness low-temperature tin-bismuth system solder, the area fraction ratio of the tin-bismuth eutectic structure to the beta-Sn phase is not obviously changed by combining the performance data of the alloy, but the plasticity of the five-element wrapped eutectic tin-bismuth system alloy is obviously improved.
TABLE 1 comparison of mechanical properties of solder alloys
TABLE 2 statistical table of alloy phase area fraction
According to the invention, the five-element-coated eutectic tin-bismuth-based solder with high toughness is obtained by the aid of alloy component design assisted by thermodynamic calculation, so that the elongation of the solder alloy is remarkably improved compared with that of SnBi58 binary alloy and SnBi55.3Sb0.81Ag0.55 quaternary-coated eutectic tin-bismuth-based alloy under the condition that the melting point, the tensile strength and the phase structure area fraction of the solder alloy are not changed, thereby improving the toughness of the solder alloy, and being beneficial to solving the problems that the toughness of the SnBi58 binary alloy is poor and the toughness of the SnBi55.3Sb0.81Ag0.55 quaternary-coated eutectic tin-bismuth-based alloy is not remarkably improved. Compared with the SnBi58 binary eutectic alloy and the SnBi55.3Sb0.81Ag0.55 quaternary coating eutectic tin-bismuth series alloy, the melting temperature is similar, the phase area fractions are basically consistent, the tensile strength difference is less than 5MPa, and the fracture elongation is improved by over 155 percent, so that the toughness is improved.
Claims (3)
1. A quinary-pack eutectic high-toughness low-temperature tin-bismuth series solder is characterized in that: the five-element-coated eutectic high-toughness tin-bismuth-series solder comprises the following components in percentage by mass: 0.431% of In, 0.019% of Cu, 0.602% of Sb and 56.86% of Bi, and the balance of Sn and inevitable impurities.
2. The preparation method of the quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth system solder as claimed in claim 1, characterized in that the preparation method comprises the following steps:
1) Preparing SnCu10 intermediate alloy;
2) Obtaining the mass percentages of all components of the five-element-coated eutectic high-toughness tin-bismuth-series solder through thermodynamic calculation, adding the SnCu10 intermediate alloy and metals Sn, bi, in and Sb according to the calculated mass percentages into a lead-free titanium-tin furnace to be melted, covering an antioxidant on the surface of the alloy, heating the alloy to 400 ℃, preserving the temperature for 30min, casting the alloy into a mold to prepare an alloy ingot, wherein the alloy undergoes the following coating eutectic reaction In the solidification process, and Liquid + SbSn = InSb + Cu 6 Sn 5 - η + (Sn) + (Bi) to obtain the five-membered eutectic high-toughness tin-bismuth-based solder, the melting temperature of which is 144.7 ℃.
3. The preparation method of the quintuple-wrapped eutectic high-toughness low-temperature tin-bismuth system solder as claimed in claim 2, characterized in that the preparation method of the SnCu10 master alloy is as follows: respectively adding Sn and Cu with the purity of 99.99wt.% into a vacuum melting furnace according to the mass ratio of 90 to 10, vacuumizing to 3 x 10-3MPa, filling nitrogen, heating to 1100 ℃ for melting, preserving heat for 30min, and then carrying out vacuum casting to prepare the SnCu10 intermediate alloy, wherein the melting point of the alloy is 450 ℃.
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