CN115401357B - Composite solder alloy containing in-situ synthesized nano reinforcing phase and preparation method thereof - Google Patents
Composite solder alloy containing in-situ synthesized nano reinforcing phase and preparation method thereof Download PDFInfo
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- CN115401357B CN115401357B CN202211052827.8A CN202211052827A CN115401357B CN 115401357 B CN115401357 B CN 115401357B CN 202211052827 A CN202211052827 A CN 202211052827A CN 115401357 B CN115401357 B CN 115401357B
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- solder alloy
- nano
- composite solder
- inorganic salt
- composite
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 83
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 77
- 239000000956 alloy Substances 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 23
- 230000003014 reinforcing effect Effects 0.000 title claims description 21
- 238000002360 preparation method Methods 0.000 title abstract description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 26
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 20
- 230000006698 induction Effects 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 238000003723 Smelting Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000003466 welding Methods 0.000 description 10
- 229910020830 Sn-Bi Inorganic materials 0.000 description 8
- 229910018728 Sn—Bi Inorganic materials 0.000 description 8
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910020922 Sn-Pb Inorganic materials 0.000 description 1
- 229910008783 Sn—Pb Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/264—Bi as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention discloses a composite solder alloy containing in-situ synthesized nano reinforced phase and a preparation method thereof, comprising a SnBi series solder alloy matrix and nano zirconium boride phases, wherein the nano zirconium boride phases are synthesized in-situ in the solder alloy matrix and dispersed; wherein the nano zirconium boride accounts for 0.5-5% of the mass of the composite solder alloy; the preparation method comprises the following steps: preparing mixed inorganic salt, preparing composite solder alloy and vacuum induction smelting; the composite solder alloy prepared by the method has fine microstructure, excellent mechanical property, excellent thermal fatigue property and creep property and low cost.
Description
Technical Field
The invention relates to a composite solder alloy containing an in-situ synthesized nano reinforcing phase and a preparation method thereof, belonging to the field of low-temperature electronic packaging materials.
Background
Sn-Bi based lead-free solder alloys have received considerable attention from researchers due to their low melting point, coefficient of thermal expansion and good wettability. The Sn-Bi-based lead-free solder can be used to prepare a solder alloy having a very wide melting temperature range by adding Bi to Sn. The alloy does not form a compound, but dissolves a large amount of Bi in a Sn matrix. The melting point of the solder alloy is lower due to the existence of Bi element; in addition, the Sn-Bi solder alloy has a wetting angle with copper of less than 45 degrees and good fluidity, so that the Sn-Bi solder alloy has good wettability with copper. In addition, the Sn-Bi alloy has good thermal expansion coefficient; under the service condition, the welding spot cracking caused by the large difference of the thermal expansion coefficients between the welding spot and the base metal can not occur. It has higher yield strength, shear strength, tensile strength and creep resistance than Sn-Pb solder at room temperature. Meanwhile, the solder has good thermal fatigue performance, no problem is caused to the welding of surface-mounted elements, and the Sn-Bi solder has low cost and can be produced in large quantity to meet the requirements. However, since the Sn-Bi-based solder segregates during solidification to form a large brittle Bi-rich phase, the Sn-Bi solder alloy exhibits characteristics of high brittleness and low ductility; bi can be separated out at the interface of the welding spot near one side of the copper plate in the service process, so that brittle failure is likely to occur when the welding spot is subjected to mechanical impact, and the performance of a welded joint is seriously affected.
Disclosure of Invention
The invention aims to provide a composite solder alloy containing an In-situ synthesized nano reinforcing phase, wherein the composite solder alloy contains In-situ generated nano reinforcing phase which is zirconium boride, and the solder alloy matrix contains Sn, bi, ag and In; the weight percentage of each component is as follows: 42% ± 0.02%, ag:1% ± 0.02%, in:1% +/-0.02%, 0.5-5% of zirconium boride and the balance Bi.
The melting characteristic of the composite solder alloy is equivalent to that of the traditional Sn-58Bi solder, and the composite solder alloy can completely adapt to a low-temperature welding process; the solder joint has excellent mechanical property and wettability, and the reliability of the soldered solder joint is good, and the solder joint can meet the development requirement of the microelectronic packaging industry, thereby being applied to the soldering of surface mount components, light-emitting diodes and the like.
Preferably, the nano reinforcing phase is generated in situ by the reaction of the mixed inorganic salt and the solder alloy matrix, the size of the nano reinforcing phase is 200-500 nm, and the nano reinforcing phase is dispersed in the solder alloy matrix.
The invention also aims to provide a preparation method of the composite solder alloy containing the in-situ synthesized nano reinforcing phase, which comprises the following specific steps:
(1) Weighing K according to a molar ratio of 1:2 2 ZrF 6 And KBF 4 Preparing mixed inorganic salt.
(2) According to ZrB 2 The mass percent in the solder alloy is calculated for the mass of the desired mixed inorganic salt.
(3) And (3) weighing Sn, bi, ag, in according to the mass percentage of the components of the composite solder alloy, weighing the mixed inorganic salt prepared in the step (1) and the metal raw material according to the calculation result of the step (2), putting the mixed inorganic salt and the metal raw material into a quartz crucible, then carrying out vacuum induction smelting, and casting the composite solder alloy into a graphite mold after the solder alloy fully reacts with the inorganic salt, thus obtaining the composite solder alloy containing nano phase.
Preferably, the inventionIn the vacuum induction smelting in the step (2), the vacuum degree of a hearth is 3 multiplied by 10 -3 Pa, the induction heating current is 15-20A.
All percentages in the present invention are by mass unless otherwise specified.
The invention has the beneficial effects that:
(1) According to the invention, the zirconium boride nano reinforcing phase is introduced into the solder alloy through the in-situ synthesis method, so that the defect that nano particles cannot be uniformly added into the alloy due to overlarge surface tension of the solder alloy is effectively overcome, and the process efficiency of preparing the composite solder alloy is greatly improved.
(2) According to the invention, the zirconium boride nano reinforcing phase is introduced into the solder alloy through the in-situ synthesis method, so that the problems of serious agglomeration and difficult dispersion of nano particles are effectively solved, the reinforcing efficiency is improved, and the application of the nano particles in the solder alloy is popularized.
(3) The invention utilizes the mixed inorganic salt and the solder alloy raw material to carry out vacuum induction smelting reaction to synthesize the nano zirconium boride particles in situ, and has the advantages of simple preparation operation and low raw material cost.
(4) The invention adopts the induction smelting furnace to smelt the solder alloy, can quickly melt the raw materials for preparing the solder alloy, and simultaneously can uniformly and comprehensively stir the melt by the induction vortex, so that the solidification structure components of the solder alloy are uniformly dispersed and synthesized nano particles in situ.
(5) The nano zirconium boride particles have small size, so that the nano zirconium boride plays roles of pinning a crystal boundary and blocking the growth of crystal grains of the solder alloy when the solder alloy is solidified, and the solder alloy has a fine and uniform tissue structure; the elongation of the as-cast solder alloy reaches 85.53 percent, which is improved by about 64 percent compared with Sn55Bi1Ag1In solder alloy. Meanwhile, the nano zirconium boride particles firmly pin dislocation at the welding point interface to block atomic diffusion in the service process of the welding point, inhibit continuous growth of an IMC layer at the welding point interface, and greatly improve interface bonding strength of the welding point and reliability in the service process.
Drawings
FIG. 1 is a DSC curve of an example;
FIG. 2 is an engineering stress-strain curve of an embodiment.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific embodiments, but the scope of the invention is not limited to the description.
A composite solder alloy containing In-situ synthesized nano reinforced phase, wherein a solder alloy matrix comprises Sn, bi, ag and In, and the mass percent of each component is Sn:42% ± 0.02%, ag:1% ± 0.02%, in:1% +/-0.02% and the balance Bi; the nano reinforcing phase is generated in situ by the reaction of mixed inorganic salt and a solder alloy matrix, the size of the nano reinforcing phase is 200-500 nm, and the nano reinforcing phase is dispersed and distributed in the solder alloy matrix, wherein the content is shown in the table 1.
The preparation method of the composite solder alloy containing the nano reinforcing phase specifically comprises the following steps:
(1) Weighing K according to a molar ratio of 1:2 2 ZrF 6 And KBF 4 Preparing mixed inorganic salt.
(2) According to ZrB 2 The mass percentage in the solder alloy is calculated as the mass of the inorganic salt to be mixed, calculated as the case where all the inorganic salt participates in the reaction.
(3) According to the mass percent of the composite solder alloy components, sn, bi, ag, in, according to the calculation result of (2), the mixed inorganic salt prepared in (1) and the metal raw material are weighed and put into a quartz crucible together, and then vacuum induction smelting is carried out, wherein the vacuum degree of a hearth is 3 multiplied by 10 -3 Pa, the induction heating current is 15-20A, and after the solder alloy fully reacts with the inorganic salt, casting the mixture into a graphite mold, thus obtaining the composite solder alloy containing the nano phase.
TABLE 1 raw material addition amounts for different samples
The mass percentages of zirconium boride in the different samples prepared in the above examples are shown in table 2:
TABLE 2 mass percent of zirconium boride in various samples, in wt%
The composite solder alloy prepared in the above example was analyzed and tested, and the performance data thereof are shown in table 3:
TABLE 3 Performance data for different samples
The melting characteristics of the different samples prepared in this example are shown in FIG. 1, the mechanical properties are shown in FIG. 2, and the analysis of Table 3 shows that. After the nano zirconium boride is generated in situ, the melting points of all samples are slightly reduced, and all samples meet the performance standard of SnBi solder alloy; the elongation of all samples is improved after the nano zirconium boride is generated in situ, and when the zirconium boride content is 3wt%, the elongation of the samples reaches 85.53%, which is improved by about 64% compared with sample 4 without zirconium boride; however, when the zirconium boride content reaches 5wt%, the elongation of the composite solder alloy is reduced; the reason for the change of the elongation is mainly that a small amount of zirconium boride is generated to refine the solder alloy structure to a small extent, so that the elongation is slightly improved; when the content of zirconium boride synthesized in situ reaches 3wt%, the microstructure refinement degree of the solder alloy is high, and meanwhile, nano-scale zirconium boride particles are used as heterogeneous nucleation points, the number of Bi-rich phases in the solder alloy is reduced, so that the extensibility of the composite solder alloy is greatly improved; however, when the zirconium boride content continues to increase, zirconium boride particles can generate an agglomeration phenomenon, and when the composite solder alloy is under tensile stress, the composite solder alloy is easy to crack at particle agglomeration positions, so that the elongation of the composite solder alloy is reduced; in addition, the synthesis of the nano zirconium boride reduces the surface tension of the solder alloy, so that the spreading rate of the embodiment is slightly improved.
Claims (3)
1. A composite solder alloy containing an in-situ synthesized nano-reinforcement phase, characterized by: the composite solder alloy contains In-situ generated nano reinforcing phase which is zirconium boride, wherein the composite solder alloy matrix contains Sn, bi, ag and In; the weight percentage of each component is as follows: 42% ± 0.02%, ag:1% ± 0.02%, in:1% +/-0.02%, 0.5-5% of zirconium boride and the balance Bi;
the nano reinforcing phase is generated in situ by the reaction of mixed inorganic salt and a solder alloy matrix, the size of the nano reinforcing phase is 200 nm-500 nm, and the nano reinforcing phase is dispersed in the solder alloy matrix.
2. The method for preparing the composite solder alloy containing the in-situ synthesized nano reinforcing phase as set forth in claim 1, which is characterized by comprising the following specific steps:
(1) Weighing K according to a molar ratio of 1:2 2 ZrF 6 And KBF 4 Preparing mixed inorganic salt;
(2) According to ZrB 2 The mass percentage of the inorganic salt in the solder alloy is calculated;
(3) And (3) weighing Sn, bi, ag, in according to the mass percentage of the components of the composite solder alloy, weighing the mixed inorganic salt prepared in the step (1) and the metal raw material according to the calculation result of the step (2), putting the mixed inorganic salt and the metal raw material into a quartz crucible, then carrying out vacuum induction smelting, and casting the composite solder alloy into a graphite mold after the solder alloy fully reacts with the inorganic salt, thus obtaining the composite solder alloy containing nano phase.
3. The method for preparing a composite solder alloy containing in-situ synthesized nano-enhanced phases according to claim 2, wherein: in the step (2), when in vacuum induction smelting, the vacuum degree of a hearth is 3 multiplied by 10 -3 Pa, the induction heating current is 15-20A.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211052827.8A CN115401357B (en) | 2022-08-31 | 2022-08-31 | Composite solder alloy containing in-situ synthesized nano reinforcing phase and preparation method thereof |
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| CN202211052827.8A CN115401357B (en) | 2022-08-31 | 2022-08-31 | Composite solder alloy containing in-situ synthesized nano reinforcing phase and preparation method thereof |
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| CN115401357A CN115401357A (en) | 2022-11-29 |
| CN115401357B true CN115401357B (en) | 2024-01-30 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5965197A (en) * | 1996-12-03 | 1999-10-12 | Lucent Technologies Inc. | Article comprising fine-grained solder compositions with dispersoid particles |
| JPH11285815A (en) * | 1998-03-31 | 1999-10-19 | Toyo Alum Kk | Solder for aluminum, aluminum printed wiring board and semiconductor integrated circuit device and method for joining aluminum member using it |
| US6205264B1 (en) * | 1998-04-14 | 2001-03-20 | Lucent Technologies Inc. | Optical assembly with improved dimensional stability |
| CN103071942A (en) * | 2013-01-05 | 2013-05-01 | 张家港市东大工业技术研究院 | Low-temperature solder matrix composite solder for synthesizing magnetic-phase particles in situ and preparation method thereof |
| CN108342606A (en) * | 2018-01-19 | 2018-07-31 | 江苏大学 | A kind of method that mischmetal improves in-situ Al-base composition tissue and performance |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6565609B2 (en) * | 2015-11-02 | 2019-08-28 | 富士通株式会社 | Electronic devices, electronic components and solder |
-
2022
- 2022-08-31 CN CN202211052827.8A patent/CN115401357B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5965197A (en) * | 1996-12-03 | 1999-10-12 | Lucent Technologies Inc. | Article comprising fine-grained solder compositions with dispersoid particles |
| JPH11285815A (en) * | 1998-03-31 | 1999-10-19 | Toyo Alum Kk | Solder for aluminum, aluminum printed wiring board and semiconductor integrated circuit device and method for joining aluminum member using it |
| US6205264B1 (en) * | 1998-04-14 | 2001-03-20 | Lucent Technologies Inc. | Optical assembly with improved dimensional stability |
| CN103071942A (en) * | 2013-01-05 | 2013-05-01 | 张家港市东大工业技术研究院 | Low-temperature solder matrix composite solder for synthesizing magnetic-phase particles in situ and preparation method thereof |
| CN108342606A (en) * | 2018-01-19 | 2018-07-31 | 江苏大学 | A kind of method that mischmetal improves in-situ Al-base composition tissue and performance |
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| Publication number | Publication date |
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| CN115401357A (en) | 2022-11-29 |
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