CN114473290A - Epoxy resin composite Sn-Bi lead-free soldering paste - Google Patents
Epoxy resin composite Sn-Bi lead-free soldering paste Download PDFInfo
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- CN114473290A CN114473290A CN202011173307.3A CN202011173307A CN114473290A CN 114473290 A CN114473290 A CN 114473290A CN 202011173307 A CN202011173307 A CN 202011173307A CN 114473290 A CN114473290 A CN 114473290A
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- free solder
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- 229910020830 Sn-Bi Inorganic materials 0.000 title claims abstract description 182
- 229910018728 Sn—Bi Inorganic materials 0.000 title claims abstract description 182
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 162
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 162
- 238000005476 soldering Methods 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 229910000679 solder Inorganic materials 0.000 claims abstract description 154
- 239000000843 powder Substances 0.000 claims abstract description 70
- 239000000203 mixture Substances 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
- 239000002184 metal Substances 0.000 claims abstract description 34
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 38
- 239000000956 alloy Substances 0.000 claims description 38
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 14
- 229920000768 polyamine Polymers 0.000 claims description 13
- 230000004907 flux Effects 0.000 claims description 12
- -1 accelerator Substances 0.000 claims description 8
- 125000002723 alicyclic group Chemical group 0.000 claims description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 7
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 239000004843 novolac epoxy resin Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims 2
- 229910052718 tin Inorganic materials 0.000 claims 1
- 238000003892 spreading Methods 0.000 abstract description 8
- 230000007480 spreading Effects 0.000 abstract description 8
- 238000009736 wetting Methods 0.000 abstract description 8
- 238000010008 shearing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 32
- 238000012360 testing method Methods 0.000 description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 230000035939 shock Effects 0.000 description 15
- 238000003756 stirring Methods 0.000 description 11
- 238000003466 welding Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 229910052733 gallium Inorganic materials 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000003679 aging effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001338 liquidmetal Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910021654 trace metal Inorganic materials 0.000 description 2
- 229910001096 P alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 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
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
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- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- BSPSZRDIBCCYNN-UHFFFAOYSA-N phosphanylidynetin Chemical compound [Sn]#P BSPSZRDIBCCYNN-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
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
- B23K35/262—Sn 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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3613—Polymers, e.g. resins
Abstract
The invention relates to an epoxy resin composite Sn-Bi lead-free soldering paste. The epoxy resin composite Sn-Bi lead-free soldering paste comprises the following components in percentage by mass: 3% -10% of epoxy resin composition; 0.001 to 1.5 percent of Ag powder; 0.001 to 0.5 percent of metal Ga; Sn-Bi lead-free solder paste, the balance; the epoxy resin composition is composed of epoxy resin, a curing agent and an accelerator according to a mass ratio of 100: 10-32: 0.5-8. The epoxy resin composite Sn-Bi lead-free solder paste has good wetting and spreading performance and high shearing strength of a soldered joint, and has obvious advantages on important technical indexes such as high-temperature high-humidity reliability, cold and hot impact reliability and the like.
Description
Technical Field
The invention relates to a brazing material in the field of metallurgy, in particular to an epoxy resin composite Sn-Bi soldering paste.
Background
With the increasing updating speed of electronic products, the requirements on electronic packaging technology, especially in the field of micro-nano connection, are higher and higher. While the micro-welding spot size is required to be smaller and smaller, the load of force, electricity and heat energy required to bear the welding part is increased day by day, so that higher and higher requirements are put on the reliability and the brazing efficiency of the brazed joint.
The research result shows that: the solder material, package substrate and underfill all contribute to the heat dissipation performance of the chip scale packaged LED. Through calculation, the influence factor of the welding material is 8.54, and therefore, the improvement of the performance of the welding material has important significance on the performance of LED products and a plurality of electronic devices and the reliability of the products.
Aiming at the particularity of LED products, the Sn-Bi solder with lower melting point is preferably selected in the manufacturing process of the solder. Although the tensile strength and the creep resistance of the Sn-Bi solder are superior to those of the Sn-Pb solder, the Sn-Bi solder has great advantages in a temperature sensitive area and outer layer soldering connection of graded packaging, the Bi-rich phase with the hard and brittle property is easy to crystallize and form thick strip-shaped/blocky irregular tissue in the cooling process of the liquid Sn-Bi solder, the brittleness of the alloy is increased along with the content of the Bi phase, the plasticity of the alloy is reduced, and the reliability of soldering points cannot meet the requirement of novel electronic product connection appearing in a new and new day.
CN109175771A discloses an epoxy resin composite Sn-Bi solder paste, and CN108971794A discloses an epoxy resin-containing composite Sn-Bi lead-free solder paste. Said invention adopts epoxy resin and Sn-Bi lead-free soldering paste to make them be combined, and utilizes the reasonable matching and optimum combination of Sn-Bi lead-free soldering paste, epoxy resin, solidifying agent and accelerating agent to prepare the invented composite Sn-Bi lead-free soldering paste with higher "welding point shear strength". However, the above-mentioned epoxy resin composite Sn — Bi solder paste still has disadvantages, and particularly, the important technical indexes such as "high temperature and high humidity reliability" and "cold and hot shock reliability" still cannot meet the increasing demand for manufacturing new electronic products which are developed at a high speed.
However, it is known that the high reliability of the solder joints is a key technical index for ensuring the long service life of the electronic devices. High solder joint reliability, in addition to high strength of the solder joint, must also have excellent reliability in high temperature, high humidity, and cold thermal shock. Thus, it is highly desirable to develop a solder paste having excellent high-temperature high-humidity reliability and thermal shock reliability.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide an epoxy resin composite Sn-Bi lead-free solder paste, which has good wetting and spreading properties, high shear strength of soldered joints, and significant advantages in important technical indexes such as high-temperature high-humidity reliability, and cold-thermal shock reliability.
In order to achieve the purpose, the invention provides an epoxy resin composite Sn-Bi lead-free soldering paste which comprises the following components in percentage by mass:
3% -10% of epoxy resin composition;
0.001 to 1.5 percent of Ag powder;
0.001 to 0.5 percent of metal Ga;
Sn-Bi lead-free solder paste, the balance;
the epoxy resin composition is composed of epoxy resin, a curing agent and an accelerator according to a mass ratio of 100: 10-32: 0.5-8.
In the epoxy resin composite Sn-Bi lead-free solder paste provided by the invention, Ag powder and metal Ga are added on the basis of the epoxy resin composition and the Sn-Bi lead-free solder paste, and the proportion of the components in the epoxy resin composition are optimized. In addition, the trace metal Ga added in the solder paste can effectively generate a 'synergistic effect' with Ag element, and the high-temperature high-humidity reliability and the cold-heat shock reliability of the epoxy resin composite solder paste are improved. As can be seen from the Ag-Ga binary phase diagram, the metal Ga and the Ag element can generate an Ag-Ga intermetallic compound, and the problem that the wettability of the soldering paste is deteriorated during reflow soldering due to the generation of stable AgCl caused by trace Cl ions and Ag ions in the soldering flux can be effectively avoided.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the epoxy resin composition is preferably 3% by mass, and the epoxy resin, the curing agent and the accelerator are preferably prepared in the following mass ratio: epoxy resin, curing agent, accelerator, Ag powder 0.001% and metal Ga 0.5%.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the epoxy resin composition is preferably 5% by mass, and the epoxy resin, the curing agent and the accelerator are preferably prepared in the following mass ratio: epoxy resin, curing agent, accelerator, Ag powder 0.1% and metal Ga 0.1%.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the epoxy resin composition is preferably 7% by mass, and the epoxy resin, the curing agent and the accelerator are preferably prepared in the following mass ratio: epoxy resin, curing agent, accelerator, Ag powder 0.5% and metal Ga 0.01%.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the epoxy resin composition is 10% by mass, and the epoxy resin, the curing agent and the accelerator are mixed by mass as follows: epoxy resin, curing agent, accelerator, Ag powder 1.5% and metal Ga 0.001%.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the epoxy resin preferably comprises at least one of NPEL-134 novolac epoxy resin, NPEL-127H bisphenol A, E44 type bisphenol A and E51 type bisphenol A.
In the epoxy resin composite Sn-Bi lead-free solder paste of the present invention, the curing agent preferably includes at least one of aromatic polyamine, alicyclic polyamine, and dicyandiamide.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the accelerator preferably comprises at least one of SH-A80, SH-A85, SH-A90 and SH-A95.
The epoxy resin composite Sn-Bi lead-free solder paste is preferably a P-containing Sn-Bi lead-free solder paste, and the Sn-Bi lead-free solder paste comprises 85-95 wt% of Sn-Bi alloy powder and the balance of soldering flux.
The Sn-Bi lead-free soldering paste can be a commercially available Sn-Bi lead-free soldering paste or a self-made Sn-Bi lead-free soldering paste.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the Sn-Bi alloy powder preferably contains 33-60% of Bi element, 0.001-0.1% of P element and the balance of Sn according to mass percentage.
The Sn-Bi alloy powder may be a commercially available Sn-Bi alloy powder or a self-made Sn-Bi alloy powder. The alloy powder sold or made by self can be prepared into Sn-Bi lead-free solder paste by adopting a conventional method.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the particle diameter of the Sn-Bi alloy powder is preferably 15-65 μm.
The epoxy resin composite Sn-Bi lead-free solder paste is characterized in that the soldering Flux is ECO Flux 823 or LFD preferably.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention is characterized in that the particle diameter of the Ag powder is preferably 15-65 μm.
The epoxy resin composite Sn-Bi lead-free solder paste provided by the invention has the advantages that the adding temperature of metal Ga is preferably 80 +/-5 ℃.
The invention has the following beneficial effects:
(1) the invention adds 3-10% of epoxy resin composition, 0.001-1.5% of Ag powder and 0.001-0.5% of Ga into Sn-Bi lead-free soldering paste to prepare the epoxy resin composite soldering paste. Compared with the existing Sn-Bi lead-free soldering paste, the soldering paste has good wetting and spreading performance, can obviously improve the shear strength and reliability of a soldered joint, particularly the high-temperature high-humidity reliability and the cold-heat shock reliability, and can be used for reflow soldering of components in the electronic industry.
(2) The curing time of the epoxy resin composite Sn-Bi lead-free soldering paste is less than 5 minutes. During reflow soldering, when the peak temperature retention time is within 5 minutes, the curing can be completed; when the peak temperature retention time is more than 5 minutes and less than 10 minutes, the solder joint strength and the solder joint shape are not affected, so that the shear strength of the solder joint of the Sn-Bi lead-free solder paste can be greatly improved by the epoxy resin cured under the reflow soldering condition, and the process requirements of batch production of different reflow soldering production lines can be met.
(3) The trace metal Ga added in the invention can effectively generate 'synergistic effect' with Ag element, and the high-temperature high-humidity reliability and the cold-heat shock reliability of the epoxy resin composite soldering paste are improved. As can be seen from the Ag-Ga binary phase diagram, the metal Ga and the Ag element can generate an Ag-Ga intermetallic compound, and the problem that the wettability of the soldering paste is deteriorated during reflow soldering due to the generation of stable AgCl caused by trace Cl ions and Ag ions in the soldering flux can be effectively avoided.
(4) The epoxy resin composite Sn-Bi soldering paste provided by the invention still has excellent wetting and spreading properties and welding spot mechanical properties after being stored for one year.
Drawings
FIG. 1 is the test results of the high temperature and high humidity aging effect rule of the solder joints of the solder pastes of example 1 and comparative example 1;
FIG. 2 is a graph showing the test results of the law of the influence of the cold-heat cycle of the solder joints of the solder pastes in example 1 and comparative example 1;
FIG. 3 is a graph showing the test results of the high temperature and high humidity aging effect rule of solder paste solder joints of example 2 and comparative example 2;
FIG. 4 is a graph showing the test results of the law of the influence of the cold and hot cycles of the solder joints of the solder pastes in the embodiment 2 and the comparative example 2;
FIG. 5 is a graph showing the test results of the high temperature and high humidity aging effect rule of solder paste solder joints of example 3 and comparative example 3;
FIG. 6 is a test result of the law of influence of the cold and hot cycles of solder joints of the solder pastes of example 3 and comparative example 3;
FIG. 7 is a graph showing the test results of the high temperature and high humidity aging effect rule of solder paste solder joints of example 4 and comparative example 4;
fig. 8 shows the test results of the law of the influence of the cold and hot cycles of the solder joints of the solder pastes in the embodiment 4 and the comparative example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In some embodiments, the present invention may employ a homemade Sn-Bi alloy powder, which is conventionally prepared as follows (i.e., Sn-Bi lead-free solder):
the material is prepared by using commercially available tin ingot, bismuth ingot, tin-phosphorus alloy and silver powder, and various element raw materials according to the required proportion, and a covering agent determined by optimized screening is added during smelting or inert gas protection is adopted for smelting and casting, so that the bar can be obtained. And remelting the smelted Sn-Bi alloy (bar), and preparing the Sn-Bi alloy into alloy powder with the particle diameter of 15-65 mu m by adopting argon protection and gas atomization powder preparation equipment.
Wherein, lead (namely Pb) is taken as an impurity element in the raw material, and the total amount (mass percentage) of the lead (namely Pb) is controlled within the range of Pb being less than or equal to 0.07 wt.% so as to meet the regulation of the national standard GB/T20422-2018 Pb-free solder of the people's republic of China (the regulation of Pb in the standard is less than or equal to 0.07 wt.%).
In some embodiments, the present invention may adopt a self-made (or commercially available) Sn-Bi lead-free solder paste, and in this case, the epoxy resin composite Sn-Bi lead-free solder paste of the present invention is prepared by the following method:
(1) adding a proper amount of ethanol or ethylene glycol into Sn-Bi alloy powder accounting for 85-95% of the mass percent and the balance of soldering Flux (such as ECO Flux 823 or LED), and stirring for 10-30 min by using a high-speed stirrer (the rotating speed is 300-1200 r/min) to obtain the Sn-Bi lead-free soldering paste.
(2) Ag powder (particle diameter of 15 μm to 65 μm) was prepared according to the method for preparing Sn-Bi alloy powder. Alternatively, it is also possible to purchase commercially available Ag powder (having a particle diameter of 15 μm to 65 μm) for use. Adding a proper amount of ethanol or ethylene glycol into the Sn-Bi lead-free soldering paste, adding Ag powder according to the proportioning requirement, and continuously stirring for more than 10min, thus finishing the addition of Ag in the Sn-Bi lead-free soldering paste.
(3) Weighing the amount of metal Ga required to be added according to the proportion requirement, respectively heating the metal Ga and the Sn-Bi lead-free soldering paste added with the Ag powder to 80 +/-5 ℃, mixing the liquid metal Ga with the Sn-Bi lead-free soldering paste added with the Ag powder, continuously stirring at a high speed for 5-10min, and cooling to finish the addition of the metal Ga (called as the Sn-Bi lead-free soldering paste containing Ag and Ga). Since the melting point of Ga is only 29.8 ℃, the boiling point is as high as 2403 ℃, and Ga is not easy to oxidize, the metal Ga can be conveniently and uniformly added into the Sn-Bi soldering paste.
(4) The epoxy resin, the curing agent and the accelerator are mixed uniformly in advance according to the ratio of the epoxy resin to the curing agent to the accelerator of 100: 10-32: 0.5-8 (namely the epoxy resin composition). And then, mixing the epoxy resin composition and the rest of the prepared Sn-Bi lead-free soldering paste containing Ag and Ga according to the proportioning requirement, adding a proper amount of ethanol or ethylene glycol, stirring for 10 min-30 min by using a high-speed stirrer (the rotating speed is 300 r/min-1200 r/min), and standing for 10min to obtain the epoxy resin composite Sn-Bi lead-free soldering paste.
Wherein the epoxy resin comprises at least one of NPEL-134 novolac epoxy resin, NPEL-127H bisphenol A, E44 type bisphenol A and E51 type bisphenol A; the curing agent comprises at least one of aromatic polyamine, alicyclic polyamine and dicyandiamide; the promoter comprises at least one of SH-A80, SH-A85, SH-A90 and SH-A95.
Wherein, in the Sn-Bi alloy powder, the Bi element content is 33 to 60 weight percent, the P content is 0.001 to 0.1 weight percent, and the balance is Sn, the product of the epoxy resin composite Sn-Bi lead-free soldering paste contains 0.001 to 1.5 weight percent of Ag, 0.001 to 0.5 weight percent of Ga, 3 to 10 weight percent of epoxy resin composition, and the balance is Sn-Bi lead-free soldering paste.
In some embodiments, according to the proportioning requirement, the Sn-Bi lead-free solder paste can also be prepared by first preparing Sn-Bi lead-free solder paste from self-made (or commercially available) Sn-Bi alloy powder, then adding epoxy resin, curing agent and accelerator to prepare Sn-Bi lead-free solder paste containing the epoxy resin composition, and then adding Ag powder and metal Ga to prepare the epoxy resin composite Sn-Bi lead-free solder paste described in the application. The epoxy resin composite Sn-Bi lead-free solder paste prepared by the embodiment has the same effect as that of the epoxy resin composite Sn-Bi lead-free solder paste prepared by adding Ag powder and metal Ga and then adding the epoxy resin composition. The specific preparation steps can be described as follows:
(1) adding a proper amount of ethanol or ethylene glycol into Sn-Bi alloy powder accounting for 85-95% of the mass percent and the balance of soldering Flux (such as ECO Flux 823 or LED), and stirring for 10-30 min by using a high-speed stirrer (the rotating speed is 300-1200 r/min) to obtain the Sn-Bi lead-free soldering paste.
(2) The epoxy resin, the curing agent and the accelerator are mixed uniformly in advance according to the ratio of the epoxy resin to the curing agent to the accelerator of 100: 10-32: 0.5-8 (namely the epoxy resin composition). And then, mixing the epoxy resin composition and the rest of the prepared Sn-Bi lead-free soldering paste according to the proportioning requirement, adding a proper amount of ethanol or ethylene glycol, stirring for 10-30 min by using a high-speed stirrer (the rotating speed is 300-1200 r/min), and standing for 10min to obtain the Sn-Bi lead-free soldering paste containing the epoxy resin composition.
(3) Ag powder (particle diameter of 15 μm to 65 μm) was prepared according to the method for preparing Sn-Bi alloy powder. Alternatively, it is also possible to purchase commercially available Ag powder (having a particle diameter of 15 μm to 65 μm) for use. Adding a proper amount of ethanol or ethylene glycol into the Sn-Bi lead-free solder paste containing the epoxy resin composition, adding Ag powder according to the proportioning requirement, and continuously stirring for more than 10min, thus finishing the addition of Ag in the Sn-Bi lead-free solder paste containing the epoxy resin composition.
(4) Weighing the amount of metal Ga required to be added according to the proportioning requirement, respectively heating the metal Ga and the Sn-Bi lead-free soldering paste added with the epoxy resin composition and the Ag powder to 80 +/-5 ℃, mixing the liquid metal Ga with the Sn-Bi lead-free soldering paste added with the epoxy resin composition and the Ag powder, continuously stirring at a high speed for 5-10min, and cooling to finish the addition of the metal Ga, thereby obtaining the epoxy resin composite Sn-Bi lead-free soldering paste. Since the melting point of Ga is only 29.8 ℃, the boiling point is as high as 2403 ℃, and Ga is not easy to oxidize, the metal Ga can be conveniently and uniformly added into the Sn-Bi soldering paste.
Wherein the epoxy resin comprises at least one of NPEL-134 novolac epoxy resin, NPEL-127H bisphenol A, E44 type bisphenol A and E51 type bisphenol A; the curing agent comprises at least one of aromatic polyamine, alicyclic polyamine and dicyandiamide; the promoter comprises at least one of SH-A80, SH-A85, SH-A90 and SH-A95.
Wherein, in the Sn-Bi alloy powder, the content of Bi element is 33 wt% -60 wt%, the content of P is 0.001 wt% -0.1 wt%, and the balance is Sn, the product epoxy resin composite Sn-Bi lead-free soldering paste contains 0.001 wt% -1.5 wt% of Ag, 0.001 wt% -0.5 wt% of Ga, 3 wt% -10 wt% of epoxy resin composition, and the balance is Sn-Bi lead-free soldering paste.
Example 1
(1) Adding a proper amount of ethanol into commercial Sn-Bi lead-free soldering paste EcoLM-C10X, adding Ag powder according to the proportioning requirement, and continuously stirring for more than 10min to complete the addition of Ag in the Sn-Bi lead-free soldering paste.
Wherein, the commercial Sn-Bi lead-free solder paste EcoLM-C10X contains 85 wt% of Sn-Bi alloy powder and the balance of soldering Flux ECO Flux 823, and in the Sn-Bi alloy powder, Bi element accounts for 55 wt% of the alloy powder, P accounts for 0.001 wt%, and the balance is Sn. The diameter of the alloy powder particles is 15 to 65 μm.
Wherein the particle diameter of the Ag powder is 15-65 μm.
(2) Weighing metal Ga, respectively heating the metal Ga and the Sn-Bi lead-free soldering paste added with Ag powder to 80 +/-5 ℃, then mixing the obtained liquid metal Ga with the Sn-Bi lead-free soldering paste added with Ag powder, continuing stirring at a high speed for 8 minutes, and cooling to finish the addition of the metal Ga in the Sn-Bi lead-free soldering paste, thereby obtaining the Sn-Bi lead-free soldering paste containing Ag and Ga.
Wherein, the melting point of Ga is only 29.8 ℃, the boiling point is as high as 2403 ℃, and Ga is not easy to be oxidized, so that the metal Ga can be conveniently and uniformly added into the Sn-Bi lead-free soldering paste by adopting the mode.
(3) The epoxy resin is formed by combining NPEL-134 novolac epoxy resin and E51 type bisphenol A according to the mass ratio of 1 to 1; the curing agent is composed of aromatic polyamine and alicyclic polyamine according to the mass ratio of 1: 2; the accelerator is composed of SH-A80 and SH-A95 according to the mass ratio of 1 to 3. Then, the epoxy resin, the curing agent and the accelerator are mixed in advance according to the ratio of the epoxy resin to the curing agent to the accelerator of 100 to 10 to 0.5, and the epoxy resin composition is obtained after uniform mixing.
(4) Mixing the epoxy resin composition and Sn-Bi lead-free soldering paste containing Ag and Ga according to the proportion requirement, adding a proper amount of ethanol, stirring for 20min by using a high-speed stirrer (the rotating speed is 500 r/min-800 r/min), and standing for 10min to obtain the epoxy resin composite Sn-Bi lead-free soldering paste.
Wherein the product of the epoxy resin composite Sn-Bi lead-free solder paste contains 0.001 wt% of Ag, 0.5 wt% of Ga, 3 wt% of epoxy resin composition and the balance of commercial Sn-Bi lead-free solder paste EcoLM-C10X.
This example 1 was evaluated for reflow, specifically, in the following two ways:
(1) when the solder paste effect was evaluated by reflow soldering, reflow soldering was performed using an R0603 chip resistor element. The specific test method comprises the following steps: and selecting an FR-4 laminated board with stable electrical insulation performance, wherein a bonding pad is made of red copper, the surface treatment process is OSP, and the welding test process is completed within 3 days after the circuit board is unsealed. Reflow soldering is carried out under the conditions that the peak temperature is 190 ℃ and the heat preservation is 5min.
And uniformly suspending and placing a cooled sample (a plurality of R0603 type sheet resistors brazed on a PCB) after reflow soldering in a KTHE-715TBS type high-temperature and high-humidity test box.
The Test parameters are determined according to JEDEC industrial standard JESD22A101 Steady State Temperature testing Bias Life Test, the high Temperature and high Humidity Test conditions are set to 85 +/-2 ℃/85 +/-2% RH, and the aging time is 168h, 500h and 1000 h.
(2) When the solder paste effect was evaluated by reflow soldering, reflow soldering was performed using an R0603 chip resistor element. The specific test method comprises the following steps: and selecting an FR-4 laminated board with stable electrical insulation performance, wherein a bonding pad is made of red copper, the surface treatment process is OSP, and the welding test process is completed within 3 days after the circuit board is unsealed. Reflow soldering is carried out under the conditions that the peak temperature is 190 ℃ and the heat preservation is 5min.
And uniformly suspending and placing a cooled sample (a plurality of R0603 type sheet resistors brazed on a PCB) after reflow soldering in a KSKC-415TBS type temperature impact test box.
According to JEDEC industrial standard JESD22A104 Temperature cycling, the Temperature thermal cycle condition is set to be (-40- +125) DEG C, each cycle period (cycle) is 70min, the high Temperature and the low Temperature respectively stay for 30min, and the cycle periods are 200 cycles, 500 cycles, 750 cycles and 1000 cycles.
Comparative example 1
The difference from example 1 is that no Ag powder, Ga metal and epoxy resin composition is added to commercial Sn-Bi lead-free solder paste EcolLM-C10X.
The reflow evaluation results of example 1 and comparative example 1 are shown in fig. 1 and 2. As can be seen from FIG. 1, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 1, the point shear strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 1 is increased from 33.77N to 48.1N, the increase is more than 42%, and after the high-temperature high-humidity aging is carried out for 1000 hours, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 1 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 1; as can be seen from FIG. 2, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 1, the shear strength of the solder joint of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 1 is increased from 33.77N to 48.1N, and the increase is more than 42%, and after the test of 1000 cycles of cold and heat shock, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 1 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 1. Therefore, the epoxy resin composite Sn-Bi soldering paste obtained in the embodiment 1 not only has good wetting and spreading performance, but also can remarkably improve the shearing strength and reliability of a soldering joint, particularly the high-temperature high-humidity reliability and the cold-heat shock reliability, and can be used for reflow soldering of components in the electronic industry.
Meanwhile, by taking an FR-4 type PCB as a test board and an 1210 sheet type resistor as a test element, reflow soldering is carried out under the conditions that the peak temperature is 190 ℃ and the temperature is kept for 5min, the welding spot shear strength of the epoxy resin composite Sn-Bi lead-free soldering paste of the embodiment 1 is improved by 8 percent compared with the highest welding spot shear strength of the embodiments disclosed in the documents CN109175771A and CN108971794A,
example 2
The difference from the embodiment 1 is that:
the commercial Sn-Bi lead-free solder paste EcolLM-C10X used contains 95 wt% of Sn-Bi alloy powder and the balance of soldering flux LFD, and in the Sn-Bi alloy powder, Bi element accounts for 60 wt% of the alloy powder, P accounts for 0.1 wt%, and the balance is Sn. The diameter of the alloy powder particles is 15 to 65 μm.
In the epoxy resin composition, the epoxy resin is E44 type bisphenol A; the curing agent is dicyandiamide; the promoter is SH-A90. The mass ratio of the epoxy resin, the curing agent and the accelerator is as follows: epoxy resin, curing agent and accelerator are 100: 32: 8.
The obtained product of the epoxy resin composite Sn-Bi lead-free solder paste contains 1.5 wt% of Ag, 0.001 wt% of Ga, 10 wt% of epoxy resin composition and the balance of commercial Sn-Bi lead-free solder paste EcoLM-C10X.
Comparative example 2
The difference from example 2 is that no Ag powder, Ga metal and epoxy resin composition is added to commercial Sn-Bi lead-free solder paste EcolLM-C10X.
The reflow evaluation results of example 2 and comparative example 2 are shown in fig. 3 and 4. As can be seen from FIG. 3, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 2, the shear strength of the solder joint of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 2 is increased from 33.77N to 50.31N, the increase is more than 48.9%, and after the aging for 1000 hours at high temperature and high humidity, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 2 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 2; as can be seen from FIG. 4, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 2, the shear strength of the solder joint of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 2 is increased from 33.77N to 50.31N, and the increase is more than 48.9%, and after the test of 1000 cycles of cold and heat shock, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 2 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 2. Therefore, the epoxy resin composite Sn-Bi solder paste obtained in the embodiment 2 not only has good wetting and spreading performance, but also can remarkably improve the shear strength and reliability of a soldered joint, particularly the high-temperature high-humidity reliability and the cold-heat shock reliability, and can be used for reflow soldering of components in the electronic industry.
Example 3
The difference from the embodiment 1 is that:
the commercial Sn-Bi lead-free solder paste EcolLM-C10X used contains 90 wt% of Sn-Bi alloy powder and the balance of soldering Flux ECO Flux 823, and in the Sn-Bi alloy powder, Bi element accounts for 58 wt% of the alloy powder, P accounts for 0.05 wt%, and the balance is Sn. The diameter of the alloy powder particles is 15 to 65 μm.
In the epoxy resin composition, the epoxy resin is a combination of NPEL-127H type bisphenol A and E44 type bisphenol A according to the mass ratio of 1: 0.5; the curing agent is a combination of aromatic polyamine, alicyclic polyamine and dicyandiamide according to the mass ratio of 1: 1; the promoter is SH-A80, SH-A85, SH-A90 and SH-A95 in a mass ratio of 1: 0.5: 1. The mass ratio of the epoxy resin, the curing agent and the accelerator is as follows: epoxy resin: curing agent: accelerator: 100: 15: 1.5.
The obtained product of the epoxy resin composite Sn-Bi lead-free solder paste contains 0.1 wt% of Ag, 0.1 wt% of Ga, 5 wt% of epoxy resin composition and the balance of commercial Sn-Bi lead-free solder paste EcoLM-C10X.
Comparative example 3
The difference from example 3 is that no Ag powder, Ga metal and epoxy resin composition is added to commercial Sn-Bi lead-free solder paste EcolLM-C10X.
The reflow evaluation results of example 3 and comparative example 3 are shown in fig. 5 and 6. As can be seen from FIG. 5, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 3, the shear strength of the solder joint of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 3 is increased from 33.77N to 50.73N, the increase is more than 50%, and after aging for 1000h at high temperature and high humidity, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 3 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 3; as can be seen from FIG. 6, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 3, the solder joint shear strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 3 is increased from 33.77N to 50.73N, and the increase is more than 50%, and after the cold-heat shock 1000cycle test, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 3 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 3. Therefore, the epoxy resin composite Sn-Bi solder paste obtained in the embodiment 3 not only has good wetting spreading performance, but also can remarkably improve the shear strength and reliability of a soldered joint, particularly the high-temperature high-humidity reliability and the cold-heat shock reliability, and can be used for reflow soldering of components in the electronic industry.
Example 4
The difference from the embodiment 1 is that:
the commercial Sn-Bi lead-free solder paste EcoRM-C10X used contains 88 wt% of Sn-Bi alloy powder and the balance of flux LFD, and the Sn-Bi alloy powder contains Bi element 56.5 wt%, P0.01 wt% and the balance of Sn. The diameter of the alloy powder particles is 15 to 65 μm.
An epoxy resin composition, wherein the epoxy resin is NPEL-134 novolac epoxy resin, NPEL-127H bisphenol A, E44 bisphenol A and E51 bisphenol A which are combined according to the mass ratio of 1: 1; the curing agent is a composition of alicyclic polyamine and dicyandiamide in a mass ratio of 1: 1; the promoter is SH-A90 and SH-A95 in a mass ratio of 2: 1. The mass ratio of the epoxy resin, the curing agent and the accelerator is as follows: epoxy resin: curing agent: accelerator: 100: 25: 6.
The obtained product of the epoxy resin composite Sn-Bi lead-free solder paste contains 0.5 wt% of Ag, 0.01 wt% of Ga, 7 wt% of epoxy resin composition and the balance of commercial Sn-Bi lead-free solder paste EcoLM-C10X.
Comparative example 4
The difference from example 4 is that no Ag powder, Ga metal and epoxy resin composition is added to commercial Sn-Bi lead-free solder paste EcolLM-C10X.
The reflow evaluation results of example 4 and comparative example 4 are shown in fig. 7 and 8. As can be seen from FIG. 7, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 4, the shear strength of the solder joint of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 4 is increased from 33.77N to 52.68N, the increase is more than 56%, and after the high-temperature high-humidity aging is carried out for 1000 hours, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 4 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 4; as can be seen from FIG. 8, compared with the Sn-Bi lead-free solder paste obtained in the comparative example 4, the solder joint shear strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 4 is increased from 33.77N to 52.68N, and the increase is more than 56%, and after the test of 1000 cycles of cold and heat shock, the solder joint strength of the epoxy resin composite Sn-Bi lead-free solder paste obtained in the example 4 is still higher than that of the Sn-Bi lead-free solder paste obtained in the comparative example 4. Therefore, the epoxy resin composite Sn-Bi solder paste obtained in example 4 not only has good wetting spreading performance, but also can significantly improve the shear strength and reliability of the soldered joint, particularly the high-temperature high-humidity reliability and the cold-heat shock reliability, and can be used for reflow soldering of components in the electronic industry.
It should be noted that the above preferred embodiments are only for illustrating the present invention, but the present invention is not limited to the above embodiments, and variations and modifications within the spirit of the present invention, which are made by those skilled in the art, are included in the protection scope of the present invention.
Claims (14)
1. The epoxy resin composite Sn-Bi lead-free soldering paste is characterized by comprising the following components in percentage by mass:
3% -10% of epoxy resin composition;
0.001 to 1.5 percent of Ag powder;
0.001 to 0.5 percent of metal Ga;
Sn-Bi lead-free solder paste, the balance;
the epoxy resin composition is composed of epoxy resin, a curing agent and an accelerator according to a mass ratio of 100: 10-32: 0.5-8.
2. The epoxy resin composite Sn-Bi lead-free solder paste as claimed in claim 1, wherein the epoxy resin composition comprises 3% by mass, and the mass ratio of the epoxy resin, the curing agent and the accelerator comprises: epoxy resin, curing agent, accelerator, Ag powder 0.001% and metal Ga 0.5%.
3. The epoxy resin composite Sn-Bi lead-free solder paste as claimed in claim 1, wherein the epoxy resin composition comprises 5% by mass, and the mass ratio of the epoxy resin, the curing agent and the accelerator comprises: epoxy resin, curing agent, accelerator, Ag powder 0.1% and metal Ga 0.1%.
4. The epoxy resin composite Sn-Bi lead-free solder paste as claimed in claim 1, wherein the epoxy resin composition comprises 7% by mass, and the mass ratio of the epoxy resin, the curing agent and the accelerator comprises: epoxy resin, curing agent, accelerator, Ag powder 0.5% and metal Ga 0.01%.
5. The epoxy resin composite Sn-Bi lead-free solder paste as claimed in claim 1, wherein the epoxy resin composition comprises 10% by mass, and the mass ratio of the epoxy resin, the curing agent and the accelerator comprises: epoxy resin, curing agent, accelerator, Ag powder 1.5% and metal Ga 0.001%.
6. The epoxy resin composite Sn-Bi lead-free solder paste of claim 1, wherein the epoxy resin comprises at least one of NPEL-134 novolac epoxy resin, NPEL-127H type bisphenol A, E44 type bisphenol a, and E51 type bisphenol a.
7. The epoxy resin composite Sn-Bi lead-free solder paste of claim 1, wherein the curing agent comprises at least one of an aromatic polyamine, an alicyclic polyamine, and a dicyandiamide.
8. The epoxy composite Sn-Bi lead-free solder paste of claim 1, wherein the accelerator comprises at least one of SH-A80, SH-A85, SH-A90 and SH-A95.
9. The epoxy composite Sn-Bi lead-free solder paste of claim 1, wherein the Sn-Bi lead-free solder paste is a P-containing Sn-Bi lead-free solder paste comprising 85 to 95 wt% of Sn-Bi alloy powder and the balance of flux.
10. The epoxy resin composite Sn-Bi lead-free solder paste of claim 9, wherein the Sn-Bi alloy powder contains 33 to 60% of Bi element, 0.001 to 0.1% of P, and the balance of Sn, in mass%.
11. The epoxy resin composite Sn-Bi lead-free solder paste of claim 10, wherein the Sn-Bi alloy powder has a particle diameter of 15 to 65 μm.
12. The epoxy resin composite Sn-Bi lead-free solder paste of claim 9, wherein the Flux is ECO Flux 823 or LFD.
13. The epoxy resin composite Sn-Bi lead-free solder paste of claim 1, wherein the Ag powder has a particle diameter of 15 to 65 μm.
14. The epoxy resin composite Sn-Bi lead-free solder paste of claim 1, wherein the addition temperature of the metal Ga is 80 ℃ ± 5 ℃.
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| CN109158793A (en) * | 2018-09-20 | 2019-01-08 | 南京航空航天大学 | Sn-Ag-Cu lead-free brazing containing Ga and Nd |
| CN109175771A (en) * | 2018-10-22 | 2019-01-11 | 南京航空航天大学 | Epoxy resin composite S n-Bi lead-free solder paste |
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| JP2004188453A (en) * | 2002-12-11 | 2004-07-08 | Harima Chem Inc | Sn-BASED SOLDER ALLOY |
| JP2005014024A (en) * | 2003-06-24 | 2005-01-20 | Toshiba Corp | Solder member, soldering material, and soldering method |
| CN107825001A (en) * | 2017-11-22 | 2018-03-23 | 张家港市东大工业技术研究院 | Tin bismuth spray printing soldering paste that a kind of silver powder particles are modified and preparation method thereof |
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