CN1389326A - Nano particle reinforced Sn-Pb based composite brazing alloy and its prepn. - Google Patents
Nano particle reinforced Sn-Pb based composite brazing alloy and its prepn. Download PDFInfo
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- CN1389326A CN1389326A CN 02125594 CN02125594A CN1389326A CN 1389326 A CN1389326 A CN 1389326A CN 02125594 CN02125594 CN 02125594 CN 02125594 A CN02125594 A CN 02125594A CN 1389326 A CN1389326 A CN 1389326A
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- tin
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- lead base
- solder
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- 239000002131 composite material Substances 0.000 title claims description 38
- 239000002105 nanoparticle Substances 0.000 title claims description 21
- 238000005219 brazing Methods 0.000 title claims description 15
- 229910020816 Sn Pb Inorganic materials 0.000 title claims description 12
- 229910020922 Sn-Pb Inorganic materials 0.000 title claims description 12
- 229910008783 Sn—Pb Inorganic materials 0.000 title claims description 12
- 229910045601 alloy Inorganic materials 0.000 title claims description 12
- 239000000956 alloy Substances 0.000 title claims description 12
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005476 soldering Methods 0.000 claims description 24
- 239000006071 cream Substances 0.000 claims description 7
- 230000002708 enhancing effect Effects 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005728 strengthening Methods 0.000 claims 1
- 229910000679 solder Inorganic materials 0.000 abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- 230000003014 reinforcing effect Effects 0.000 abstract 3
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 15
- 238000013019 agitation Methods 0.000 description 10
- 239000006023 eutectic alloy Substances 0.000 description 10
- 230000005496 eutectics Effects 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 230000007480 spreading Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 240000006409 Acacia auriculiformis Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000000050 ionisation spectroscopy Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention relates to a nano granule reinforced tin-lead base compound solder and its preparation method. It is formed from granular tio-lead base body and nano granular reinforcing body through mixing process, and is characterized by that the described granular tin-lead base body size is 35-75 micrometers, in which tin content is 60-65 wt%, Ce base mixed rare earth content is 0-0.3 wt% and the rest is lead, the described nano granular reinforcing body incldues TiO2, Al2O3, industrial pure Ag or Cu, its size is 25-90 nm, and its volume ratio in the compound solder is 0.5-5%. The above-mentioned granular tin-lead base body, nano granular reinforcing body and neutral scaling powder are uniformly mixing, stirred for 30-40 min so as to obtain the invented compound solder paste.
Description
One, technical field
Sn-Pb based composite brazing alloy that a kind of nano particle strengthens and preparation method thereof belongs to the metal-base composites technical field.
Two, background technology
Tin-lead solder is widely used in electronics industry, realize in the components and parts and components and parts and printed circuit board (PCB) between be electrically connected and mechanical connection.Along with the miniaturization of components and parts and the development of surface installation technique, more and more higher to the requirement of microstructure stability, the mechanical property, particularly creep-resistant property of solder.
Near the automobile engine, the environment temperature in winter can be in the fluctuation of-40 ℃ to 200 ℃ scopes, and automotive electronics will stand repeatedly thermal cycling stresses, the accidental impact that also will absorb the shock loads on engine and road surface and drive to run into solder.As time goes on being connected and fixed of optical fiber in optical cable project, if the axle vertical plane of optical fiber departs from centering gradually because of creep, will cause the reduction of signal intensity in transmission.In the photoelectron assembling, as the coupling between the globe lens of solid state laser chip and optical fiber, its coupling efficiency depends on the accurate centering of the axle vertical plane of optical fiber.Being positioned in the whole service life-span between the element must keep accurately, any displacement that causes because of creep, all may influence the transmission quality of optical signal, even the transmission signal is completely lost, in fact this depend on the croop property of solder or the dimensional stability of junction.Therefore, on the basis that keeps the tin-lead solder superperformance, it is very important to improve its creep resistance.Compare with conventional telecommunication and data communication, military and aerospace electronic equipment requires optic module to be on active service under adverse circumstances such as vibrations, acceleration for a long time, and the creep-resistant property of solder also requires higher.
At present, extensively adopt the auri solder in the photoelectron assembling, as the 80Au-20Sn eutectic solder, though this solder creep resistance is higher, solder fusing point higher (273 ℃) in brazing process, often causes the damage of optical fiber or opto-electronic device, and costs an arm and a leg.
Plumbous eutectic of tin or nearly eutectic solder fusing point lower (183 ℃), cheap, the soldering processes performance is good, but creep-resistant property is poor.The lead-free solder of present exploitation, though the creep-resistant property of some lead-free solders is better than tin-lead solder, the fusion temperature of these lead-free brazings generally is higher than about 40 ℃ of the plumbous eutectic solder of tin.
The AT﹠T Labs of U.S. Lucent in 1998 adds aluminium oxide or TiOx nano particle in the 63Sn-37Pb eutectic solder, size is respectively 10nm and 5nm, and adding volume ratio is 3%, makes composite through rolling repeatedly.The composite block that is of a size of 3.5mm * 3.5mm * 4.5mm is done dead load compression creep rate test, the result shows that the incompressible croop property of this composite is better than the 80Au-20Sn brazing filler metal alloy, but whether do not do the performance test after the material fusing and the test of desired physical properties and processing performance when using as solder, promptly not drawing can be as the data of solder use.
Three, summary of the invention
The object of the present invention is to provide Sn-Pb based composite brazing alloy of a kind of creep-resistant property height, the simple nano particle enhancing of preparation method and preparation method thereof.
The Sn-Pb based composite brazing alloy that nano particle provided by the present invention strengthens strengthens body by granular tin lead base body and Nanoparticulate and is mixed and made into, it is characterized in that: described granular tin lead base body size is between 35-75 μ m, wherein the percentage by weight of tin is 60-65%, the percentage by weight of Ce base mishmetal is 0-0.3%, and all the other are plumbous; It is TiO that described Nanoparticulate strengthens body
2, Al
2O
3Metal oxide, technical pure metal A g or Cu, nominal size is between 25-90nm, and the volume ratio in composite soldering is 0.5-5%.
The preparation method of the Sn-Pb based composite brazing alloy that nano particle provided by the invention strengthens, it is characterized in that:, stir 30-40min and make composite soldering cream by above-mentioned granular tin lead base body, Nanoparticulate being strengthened body and the evenly mixing of neutral scaling powder machinery.
For the size and the cooling condition of simulating actual electronics jointing, the test specimen that adopts in creep test is miniature single-ride joint, and the overlap joint area of soldered fitting is 1mm
2, brazed seam thickness is 0.15mm, and being connected material is red copper foil, and thickness is 0.1mm.In order to compare the croop property that nano particle strengthens composite soldering and common tin lead solder, employing is drawn and is cut test creep life, and test is carried out under the dead load stretching condition, and it is 11.27Mpa that the perseverance of test specimen is drawn shear stress, test temperature is 15 ℃, and the time of breaking of sample is its creep life.Spreading area test is with reference to National Standard solder spreadability and joint filling experimental technique " regulation of GB11364-89.Substrate is the thick scale copper of 0.2mm, is of a size of 40mm * 40mm.The Cu paper tinsel is through No. 600 sand paperings, and absolute ethyl alcohol cleans airing.Solder paste weight is 0.227g.Weighing Sai Duolisi electronic balance.Sprawl soldering test with HZ-3C computer control Re-current welder, carry out in the air.The Sn-Pb based composite brazing alloy sample that five kinds of nano particles strengthen among the embodiment and 63Sn-37Pb solder sample all are preparations and testing under above-mentioned identical condition.Other test event comprises: hot strength, fusion temperature, electrical conductivity etc.
Nano particle strengthens the result of the test of Sn-Pb based composite brazing alloy performance and sees attached list, result of the test shows: nano particle enhancing Sn-Pb based composite brazing alloy fusion temperature is low, better (spreading area is bigger for wetability, angle of wetting is less), advantage such as tensile strength and physical property be good, the composite soldering joint that nano particle strengthens is bigger creep life, and creep-resistant property is better.
Four, specific embodiment
Embodiment 1: the matrix that nano particle strengthens the plumbous composite soldering of tin is the nearly eutectic alloy of 60Sn-40Pb, and nominal size is 35 μ m, and the percentage by weight that contains Ce base mishmetal is 0.1%.It is Al that Nanoparticulate strengthens body
2O
3Nano-oxide particles, handle through anti-agglomeration on the surface, and nominal size is 90nm, and the volume ratio in composite soldering is 0.5%.Take by weighing the Al of 0.024g
2O
3Exempt to clean neutral scaling powder with above-mentioned mishmetal of 0.01g and 1.36g, put into crucible mechanical agitation 30min, to be mixed evenly after, add the nearly eutectic alloy of 60Sn-40Pb of 10g, mechanical agitation 30min makes composite soldering cream, low temperature is preserved standby.
Embodiment 2: the matrix that nano particle strengthens the plumbous composite soldering of tin is the 63Sn-37Pb eutectic alloy, and nominal size is 43 μ m.It is rutile-type oxide TiO that Nanoparticulate strengthens body
2, handle through anti-agglomeration on the surface, and nominal size is 70nm, and the volume ratio in composite soldering is 3%.Take by weighing the TiO of 0.158g
2Exempt to clean neutral scaling powder with 1.36g, put into crucible mechanical agitation 40min, to be mixed evenly after, add the 63Sn-37Pb eutectic alloy of 10g, mechanical agitation 30min makes composite soldering cream, low temperature is preserved standby.
Embodiment 3: the matrix that nano particle strengthens the plumbous composite soldering of tin is the nearly eutectic alloy of 65Sn-35Pb, and nominal size is 75 μ m, and the percentage by weight that contains Ce base mishmetal is 0.3%.It is anatase titanium dioxide oxide TiO that Nanoparticulate strengthens body
2, handle through anti-agglomeration on the surface, and nominal size is 50nm, and the volume ratio in composite soldering is 5%.Take by weighing the TiO of 0.269g
2Exempt to clean neutral scaling powder with above-mentioned mishmetal of 0.03g and 1.36g, put into crucible mechanical agitation 30min, to be mixed evenly after, add the nearly eutectic alloy of 65Sn-35Pb of 10g, mechanical agitation 35min makes composite soldering cream, low temperature is preserved standby.
Embodiment 4: the matrix that nano particle strengthens the plumbous composite soldering of tin is the 63Sn-37Pb eutectic alloy, and nominal size is 43 μ m.It is simple metal Ag that Nanoparticulate strengthens body, and purity is 99.9%, and nominal size is 35nm, and the volume ratio in composite soldering is 3%.The Ag and the 1.36g that take by weighing 0.389g exempt to clean neutral scaling powder, put into crucible mechanical agitation 35min, to be mixed evenly after, add the 63Sn-37Pb eutectic alloy of 10g, mechanical agitation 30min makes composite soldering cream, low temperature is preserved standby.
Embodiment 5: the matrix that nano particle strengthens the plumbous composite soldering of tin is the 63Sn-37Pb eutectic alloy, and nominal size is 43 μ m.It is simple metal Cu that Nanoparticulate strengthens body, and purity is 99.9%, and nominal size is 25nm, and the volume ratio in composite soldering is 3%.The Cu and the 1.36g that take by weighing 0.329g exempt to clean neutral scaling powder, put into crucible mechanical agitation 30min, to be mixed evenly after, add the 63Sn-37Pb eutectic alloy of 10g, mechanical agitation 40min makes composite soldering cream, low temperature is preserved standby.The Sn-Pb based composite brazing alloy performance test table that the nano particle of subordinate list: embodiment 1 to 5 strengthens
Embodiment | Fusing point (℃) | Tensile strength (MPa) | Spreading area (mm 2) | Angle of wetting (°) | Surface tension (MN/m) | Electrical conductivity (%ICAS) | Relative creep life |
??63Sn37Pb | ??183 | ??35.5 | ??106.1 | ??5.7 | ??468 | ??12.28 | ??1 |
Embodiment 1 | ??183-190 | ??43.7 | ??106.6 | ??7.3 | ??469 | ??12.31 | ??7.0 |
Embodiment 2 | ??183 | ??46.2 | ??112.7 | ??7.2 | ??469 | ??12.17 | ??4.8 |
Embodiment 3 | ??183-186 | ??47.5 | ??109.1 | ??7.7 | ??469 | ??12.05 | ??4.4 |
Embodiment 4 | ??183 | ??34.6 | ??98.8 | ??6.2 | ??468 | ??12.62 | ??40 |
Embodiment 5 | ??183 | ??48.0 | ??81.8 | ??6.9 | ??469 | ??12.98 | ??6.5 |
* relative creep life: be 1 the creep life of establishing 63Sn37Pb eutectic solder joint, the expression nano particle strengthens composite soldering joint creep life relatively its creep life multiple.(solder connector creep test specimen is 12).
Claims (2)
1, a kind of Sn-Pb based composite brazing alloy of nano particle enhancing, strengthening body by granular tin lead base body and Nanoparticulate is mixed and made into, it is characterized in that: described granular tin lead base body size is between 35-75 μ m, wherein the percentage by weight of tin is 60-65%, the percentage by weight of Ce base mishmetal is 0-0.3%, and all the other are plumbous; It is TiO that described Nanoparticulate strengthens body
2, Al
2O
3Metal oxide, technical pure metal A g or Cu, nominal size is between 25-90nm, and the volume ratio in composite soldering is 0.5-5%.
2, a kind of preparation method of Sn-Pb based composite brazing alloy of nano particle enhancing is characterized in that: by above-mentioned granular tin lead base body, Nanoparticulate being strengthened body and the evenly mixing of neutral scaling powder machinery, stirring 30-40min makes composite soldering cream.
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CNB021255946A CN1152769C (en) | 2002-07-24 | 2002-07-24 | Nano particle reinforced Sn-Pb based composite brazing alloy and its prepn. |
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CN1152769C CN1152769C (en) | 2004-06-09 |
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Cited By (16)
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CN100469222C (en) * | 2003-12-22 | 2009-03-11 | 罗姆和哈斯电子材料有限责任公司 | Methods of forming solder areas on electronic components and electronic components having solder areas |
CN100471364C (en) * | 2003-12-22 | 2009-03-18 | 罗姆和哈斯电子材料有限责任公司 | Electronic devices and methods of forming electronic devices |
US20090301606A1 (en) * | 2005-05-25 | 2009-12-10 | Minoru Ueshima | Lead-free solder paste |
CN101823187B (en) * | 2010-02-04 | 2012-01-25 | 哈尔滨工业大学 | Nano-Ni reinforced low-temperature lead-free composite solder paste and preparation method thereof |
CN103203563A (en) * | 2013-04-08 | 2013-07-17 | 上海大学 | Strengthened composite lead-free solder containing nanometer TiO2 particles |
CN104588903A (en) * | 2014-12-08 | 2015-05-06 | 北京康普锡威科技有限公司 | Ag2O-particle-reinforced tin-lead-based composite solder and preparation method thereof |
CN105057911A (en) * | 2015-08-26 | 2015-11-18 | 华南理工大学 | Tin-silver-copper composite solder paste enhanced by titanium dioxide nanoparticles and preparation method thereof |
CN105364243A (en) * | 2015-11-26 | 2016-03-02 | 芜湖雅葆轩电子科技有限公司 | Signal processing base board |
CN105364341A (en) * | 2015-11-26 | 2016-03-02 | 芜湖雅葆轩电子科技有限公司 | Signal processing base board |
CN105364340A (en) * | 2015-11-26 | 2016-03-02 | 芜湖雅葆轩电子科技有限公司 | Solder paste for signal processing base board and preparation method of solder paste |
CN105397343A (en) * | 2015-11-26 | 2016-03-16 | 芜湖雅葆轩电子科技有限公司 | Solder paste for signal processing substrate and preparation method thereof |
CN105779815A (en) * | 2016-03-18 | 2016-07-20 | 苏州莱特复合材料有限公司 | Aluminum oxide particle reinforced lead-base composite material and preparation method thereof |
CN110323449A (en) * | 2018-03-28 | 2019-10-11 | Jx金属株式会社 | Lithium ion battery current collector rolled copper foil and lithium ion battery |
CN110508973A (en) * | 2019-09-11 | 2019-11-29 | 重庆群崴电子材料有限公司 | High-temperature service solder(ing) paste and preparation method thereof is realized in a kind of doping of nano particle |
CN110653516A (en) * | 2019-10-31 | 2020-01-07 | 深圳群崴半导体材料有限公司 | Special soldering paste for welding multistage packaging patch elements |
CN110961826A (en) * | 2019-12-25 | 2020-04-07 | 哈尔滨工业大学 | Preparation method of nano IMC (internal mold decoration) uniformly-reinforced tin-based alloy joint |
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CN100469222C (en) * | 2003-12-22 | 2009-03-11 | 罗姆和哈斯电子材料有限责任公司 | Methods of forming solder areas on electronic components and electronic components having solder areas |
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US20090301606A1 (en) * | 2005-05-25 | 2009-12-10 | Minoru Ueshima | Lead-free solder paste |
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CN103203563A (en) * | 2013-04-08 | 2013-07-17 | 上海大学 | Strengthened composite lead-free solder containing nanometer TiO2 particles |
CN104588903A (en) * | 2014-12-08 | 2015-05-06 | 北京康普锡威科技有限公司 | Ag2O-particle-reinforced tin-lead-based composite solder and preparation method thereof |
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CN105057911A (en) * | 2015-08-26 | 2015-11-18 | 华南理工大学 | Tin-silver-copper composite solder paste enhanced by titanium dioxide nanoparticles and preparation method thereof |
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CN105779815A (en) * | 2016-03-18 | 2016-07-20 | 苏州莱特复合材料有限公司 | Aluminum oxide particle reinforced lead-base composite material and preparation method thereof |
CN110323449A (en) * | 2018-03-28 | 2019-10-11 | Jx金属株式会社 | Lithium ion battery current collector rolled copper foil and lithium ion battery |
CN110508973A (en) * | 2019-09-11 | 2019-11-29 | 重庆群崴电子材料有限公司 | High-temperature service solder(ing) paste and preparation method thereof is realized in a kind of doping of nano particle |
CN110508973B (en) * | 2019-09-11 | 2021-07-06 | 重庆群崴电子材料有限公司 | High-temperature service soldering paste realized by doping nano particles and preparation method thereof |
CN110653516A (en) * | 2019-10-31 | 2020-01-07 | 深圳群崴半导体材料有限公司 | Special soldering paste for welding multistage packaging patch elements |
CN110653516B (en) * | 2019-10-31 | 2022-02-15 | 深圳群崴半导体材料有限公司 | Special soldering paste for welding multistage packaging patch elements |
CN110961826A (en) * | 2019-12-25 | 2020-04-07 | 哈尔滨工业大学 | Preparation method of nano IMC (internal mold decoration) uniformly-reinforced tin-based alloy joint |
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