CN101817127A - Sn-58Bi lead-free solder reinforced by carbon nano tube and preparation method thereof - Google Patents
Sn-58Bi lead-free solder reinforced by carbon nano tube and preparation method thereof Download PDFInfo
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- CN101817127A CN101817127A CN 201010167210 CN201010167210A CN101817127A CN 101817127 A CN101817127 A CN 101817127A CN 201010167210 CN201010167210 CN 201010167210 CN 201010167210 A CN201010167210 A CN 201010167210A CN 101817127 A CN101817127 A CN 101817127A
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Abstract
The invention relates to an Sn-58Bi lead-free solder reinforced by a carbon nano tube and a preparation method thereof, in particular to a low-temperature solder and the preparation method thereof, which solves the problem that the plasticity of Sn-58Bi alloy is lowered owing to the frangibility of BI to affect the property of welding joints. TheSn-58Bi lead-free solder reinforced by the carbon nano tube is prepared from eutectic Sn-58Bi alloy powder, the carbon nano tube and soldering flux. The preparation method comprises the following steps: ball-milling the eutectic Sn-58Bi alloy powder and the carbon nano tube under the protection of argon to obtain solder powder; and uniformly mixing the solder powder with the soldering flux, and then smelting and air-cooling to obtain the reinforced Sn-58Bi lead-free solder. In the invention, the maximum bending strength of the Sn-58Bi lead-free solder reinforced by the carbon nano tube is 184.12MPa, improved by 10% than that of Sn-58Bi solder alloy; the elongation is improved by about 48.9% than that of the Sn-58Bi solder alloy; and compared with the original solder, the quantity of the welding spots with tensile strength distributed in 11-15N is improved by 52.2%.
Description
Technical field
The present invention relates to a kind of low-temperature leadless solder and preparation method thereof.
Background technology
With the Sn-58Bi alloy is that the solder of representing has special advantages in the application of low temperature encapsulation.But make that Sn-58Bi alloy fragility is big because Bi itself is very crisp, ductility is little.Bi easy crystallization in alloy forms thick irregular shape, particularly alligatoring is more serious when long term high temperature is worked, and causes alloy plasticity to reduce, even brittle break occurs, thereby have a strong impact on property of welded joint, the fragility that therefore reduces alloy is the problem that presses for solution.
Summary of the invention
The objective of the invention is to reduce, influence the problem of property of welded joint, a kind of Sn-58 Bi lead-free solder reinforced by carbon nano tube and preparation method thereof is provided in order to solve the very crisp Sn-58Bi of the making alloy plasticity of Bi itself.
Sn-58 Bi lead-free solder reinforced by carbon nano tube of the present invention is ball milling under argon shield with eutectic Sn-58Bi alloyed powder and CNT; then mixture is added scaling powder and carry out melting; air cooling is made; wherein the mass fraction of CNT is 0.01%～0.1% in the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling, and the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling and the mass ratio of scaling powder are 8 ﹕ 2.
The preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube is as follows: one, with eutectic Sn-58Bi alloyed powder and CNT under argon shield, with the rotating speed ball milling 50min of 300r/min, obtain the CNT mass fraction and be 0.01%～0.1% solder powder; Two, solder powder and scaling powder are mixed the back according to the mass ratio of 8 ﹕ 2 and be incubated 60s～80s melting under 170 ℃～180 ℃ condition, air cooling promptly gets Sn-58 Bi lead-free solder reinforced by carbon nano tube.
The granularity of above-mentioned eutectic Sn-58Bi alloyed powder is 25 μ m～75 μ m; Above-mentioned scaling powder is Flux55.
Sn-58 Bi lead-free solder reinforced by carbon nano tube bending strength of the present invention is up to 184.12MPa, compares with the bending strength (167.68MPa) of Sn-58Bi brazing filler metal alloy, and its bending strength has improved 10%.The percentage elongation of Sn-58 Bi lead-free solder reinforced by carbon nano tube (21.68%) is compared with the percentage elongation (14.56%) of Sn-58Bi brazing filler metal alloy and has nearly been improved 48.90%.Pull-off strength test at reflowed solder joint shows that compare with original solder, Sn-58 Bi lead-free solder reinforced by carbon nano tube tensile strength has improved 52.2% in the number of welds that is distributed in 11～15N.
Description of drawings
Fig. 1 is the SEM shape appearance figure of the used CNT of the present invention; Fig. 2 is a three point bending test schematic diagram in the specific embodiment 13; Fig. 3 is a three point bending test schematic diagram in the specific embodiment 13; Fig. 4 is a tensile sample schematic diagram in the specific embodiment 13; Fig. 5 is the shape appearance figure of observed CNT in the stretching fracture in the specific embodiment 13; Fig. 6 is a pull-off strength verification test schematic diagram in the specific embodiment 13; Fig. 7 is the figure of tissue topography of the used Sn-58Bi solder of the present invention; Fig. 8 is the figure of tissue topography of gained Sn-58 Bi lead-free solder reinforced by carbon nano tube (Sn-58Bi-0.03CNTs) in the specific embodiment 13.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: Sn-58 Bi lead-free solder reinforced by carbon nano tube is ball milling under argon shield with eutectic Sn-58Bi alloyed powder and CNT in the present embodiment; then mixture is added scaling powder and carry out melting; air cooling is made; wherein the mass fraction of CNT is 0.01%～0.1% in the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling, and the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling and the mass ratio of scaling powder are 8 ﹕ 2.The mass fraction of Sn is 42% in the described eutectic Sn-58Bi alloyed powder, and the mass fraction of Bi is 58%.
Used CNT is a multi-walled carbon nano-tubes in the present embodiment.
CNT (FloTube9000) used in the present embodiment is provided by sky Nai Nami (Cnano) Co., Ltd, and the used ball mill of ball milling is the QM-1SP type planetary ball mill that Nanjing Univ. Instrument Factory produces.
The specific embodiment two: present embodiment and the specific embodiment one are different is that the granularity of described eutectic Sn-58Bi alloyed powder is 25 μ m～75 μ m.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different with one of the specific embodiment one or two is that described scaling powder is Flux55.Other is identical with one of the specific embodiment one or two.
The specific embodiment four: present embodiment is different with one of specific embodiment one to three is that the mass fraction of CNT is 0.04%～0.08% in the mixture behind described eutectic Sn-58Bi alloyed powder and the CNT ball milling.Other is identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different with one of specific embodiment one to four is that the mass fraction of CNT is 0.06% in the mixture behind described eutectic Sn-58Bi alloyed powder and the CNT ball milling.Other is identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different with one of specific embodiment one to five is that the mass fraction of CNT is 0.03% in the mixture behind described eutectic Sn-58Bi alloyed powder and the CNT ball milling.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube is as follows in the present embodiment: one, with eutectic Sn-58Bi alloyed powder and CNT under argon shield, with the rotating speed ball milling 50min of 300r/min, obtain the CNT mass fraction and be 0.01%～0.1% solder powder; Two, solder powder and scaling powder are mixed the back according to the mass ratio of 8 ﹕ 2 and be incubated 60s～80s melting under 170 ℃～180 ℃ condition, air cooling promptly gets Sn-58 Bi lead-free solder reinforced by carbon nano tube.The mass fraction of Sn is 42% in the Sn-58Bi of eutectic described in the step 1 alloyed powder, and the mass fraction of Bi is 58%.
Used CNT is a multi-walled carbon nano-tubes in the present embodiment.
CNT (FloTube9000) used in the present embodiment is provided by sky Nai Nami (Cnano) Co., Ltd, and the used ball mill of ball milling is the QM-1SP type planetary ball mill that Nanjing Univ. Instrument Factory produces.
The tensile strength of present embodiment gained Sn-58 Bi lead-free solder reinforced by carbon nano tube and Sn-58Bi solder and percentage elongation such as table 1:
The result such as the table 2 of the bend test performance test of present embodiment gained Sn-58 Bi lead-free solder reinforced by carbon nano tube and Sn-58Bi solder:
It is little to be found out that by table 1 and table 2 Sn-58 Bi lead-free solder reinforced by carbon nano tube that has added CNT is compared its tensile strength change with the Sn-58Bi solder, but percentage elongation and bending strength all are significantly improved.
The specific embodiment eight: present embodiment and the specific embodiment one are different is that the granularity of the Sn-58Bi of eutectic described in step 1 alloyed powder is 25 μ m～75 μ m.Other is identical with the specific embodiment one.
The specific embodiment nine: what present embodiment was different with one of the specific embodiment seven or eight is that scaling powder described in the step 2 is Flux55.Other is identical with one of the specific embodiment seven or eight.
The specific embodiment ten: present embodiment is different with one of specific embodiment seven to nine be described in the step 1 in the solder powder CNT mass fraction be 0.06%.Other is identical with one of specific embodiment seven to nine.
The specific embodiment 11: present embodiment is different with one of specific embodiment seven to ten be described in the step 1 in the solder powder CNT mass fraction be 0.04%～0.08%.Other is identical with one of specific embodiment seven to ten.
The specific embodiment 12: present embodiment is different with one of specific embodiment seven to ten be described in the step 1 in the solder powder CNT mass fraction be 0.03%.Other is identical with one of specific embodiment seven to ten.
The specific embodiment 13: the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube is as follows in the present embodiment: one, with eutectic Sn-58Bi alloyed powder and CNT under argon shield, with the rotating speed ball milling 50min of 300r/min, obtain the CNT mass fraction and be 0.03% solder powder; Two, solder powder and scaling powder are incubated the 60s melting according to the mass ratio of 8 ﹕ 2 under 180 ℃ condition, air cooling promptly gets Sn-58 Bi lead-free solder reinforced by carbon nano tube (Sn-58Bi-0.03CNTs).
The Sn-58 Bi lead-free solder reinforced by carbon nano tube of present embodiment preparation is carried out following performance test:
(a) melting brazing filler metal alloy line is cut into the three-point bending sample, be of a size of length and width and height and be respectively 21mm, 4.5mm, 0.6mm.Three point bending test schematic diagram such as Fig. 2, shown in Figure 3.Used test apparatus is the INSTRONMODEL1186 electronic universal tester, and rate of head movement is 2mm/min.
The Sn-58 Bi lead-free solder reinforced by carbon nano tube bending strength of present embodiment preparation is up to 184.12MPa, compares with the bending strength (167.68MPa) of Sn-58Bi brazing filler metal alloy under the identical preparation condition, and its bending strength has improved 10%.By Fig. 7 and Fig. 8 as can be known the dendrite primary phase quantity of the black in the Sn-58Bi-0.03CNTs tissue obviously reduce, structural constituent is even, and the obvious refinement of alloy organizing, the bending strength of composite soldering raises.
(b) melting brazing filler metal alloy line is cut into tensile sample, dimensional units is mm, and the tensile sample schematic diagram as shown in Figure 4.Used test apparatus is the INSTRONMODEL1186 electronic universal tester, and rate of extension is 1mm/min.
The tensile strength (94.42MPa) of the Sn-58 Bi lead-free solder reinforced by carbon nano tube of present embodiment preparation is compared with the tensile strength (91.65MPa) of Sn-58Bi and is improved DeGrain, but the percentage elongation (21.68%) of the Sn-58 Bi lead-free solder reinforced by carbon nano tube of present embodiment preparation is compared with the percentage elongation (14.56%) of Sn-58Bi brazing filler metal alloy and is significantly improved, and has nearly improved 48.90%.
Fig. 5 is the shape appearance figure of observed CNT in the stretching fracture.From then on figure can observe the cracking that CNT has stoped crystal boundary, has improved the intensity and the toughness of brazing filler metal alloy.This is because the CNTs particle that dislocation runs into nanoscale is at the volley hindered, CNTs will dislocation line be subjected to walk around particle after curved and continue motion.If continue moving, dislocation then needs bigger stress, the moving of so further inhibition dislocation, and this will improve the yield strength of Sn-58 Bi lead-free solder reinforced by carbon nano tube.At room temperature, the thermal coefficient of expansion CTE of Sn-58Bi solder
Sn-58BiBe-1.5 * 10
-6/ K, the then very little relatively (CTE of the thermal coefficient of expansion of CNTs
CNTsBe-5.86 * 10
-9/ K).There is good bonding in the interface of CNTs and Sn-58Bi brazing filler metal alloy, so the low CTE of CNTs can suppress the expansion of matrix Sn-58Bi.In addition, the thermal expansion coefficient difference that exists between CNTs and the Sn-58Bi solder can cause in dislocation punching at the interface, and makes matrix material produce work hardening, and the intensity of brazing filler metal alloy is improved.
(c) the test substrate adopts FR-4 single face rigid plate, and thickness is 2.2mm, and selecting pad coating for use is Cu.Pcb board cleans with acetone before the soldering paste printing, removes the surface impurity dirt, and the stainless steel pringting version thickness that printing is used is 0.12mm.
With the Sn-58 Bi lead-free solder reinforced by carbon nano tube and the Sn-58Bi solder of present embodiment preparation is the alloy coat of 0.12mm with electric iron coating thickness on the Cu pad respectively, and sticks the QPF components and parts with the stainless steel pringting version behind its surface brush last layer scaling powder (Flux55).
The used pull-off test machine of present embodiment is the sub-tensile testing machine of microcomputer controlled electro, and model is KD-0.5.Get the close solder joint of form and do the pull-off strength test.Select for use QPF component down-lead spacing less because of test, select for use crochet hook can't directly extend into the test of lead-in wire shoulder, therefore can only begin test from edge from the space between two lead-in wires.After to first solder joint test of edge, its lead-in wire of breaking is fractureed, be beneficial to next solder joint is tested.
The components and parts that will test are fixed on the workbench of miter angle inclination, as shown in Figure 6.Fixedly metacoxal plate and vertical direction are miter angle; Tangle the lead-in wire shoulder with pinhock, vertically the test speed with 5mm/min upwards hooks pin, ruptures after solder joint reaches maximum load.
The pull-off strength distribution situation of the distributed data table 3(reflow welding solder joint by the solder joint load value) as can be seen, in the solder joint of being tested, compare with original solder, the number of welds that Sn-58 Bi lead-free solder reinforced by carbon nano tube solder joint tensile strength is distributed in 11～15N has improved 52.2%.
Table 3
Claims (10)
1. Sn-58 Bi lead-free solder reinforced by carbon nano tube; it is characterized in that described Sn-58 Bi lead-free solder reinforced by carbon nano tube is ball milling under argon shield with eutectic Sn-58Bi alloyed powder and CNT; then mixture is added scaling powder and carry out melting; air cooling is made; wherein the mass fraction of CNT is 0.01%～0.1% in the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling, and the mixture behind eutectic Sn-58Bi alloyed powder and the CNT ball milling and the mass ratio of scaling powder are 8 ﹕ 2.
2. Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 1, the granularity that it is characterized in that described eutectic Sn-58Bi alloyed powder are 25 μ m～75 μ m.
3. Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 1 and 2 is characterized in that described scaling powder is Flux55.
4. Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 3 is characterized in that the mass fraction of CNT in the mixture behind described eutectic Sn-58Bi alloyed powder and the CNT ball milling is 0.06%.
5. Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 3 is characterized in that the mass fraction of CNT in the mixture behind described eutectic Sn-58Bi alloyed powder and the CNT ball milling is 0.03%.
6. the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube, the preparation method who it is characterized in that Sn-58 Bi lead-free solder reinforced by carbon nano tube is as follows: one, with eutectic Sn-58Bi alloyed powder and CNT under argon shield, with the rotating speed ball milling 50min of 300r/min, obtain the CNT mass fraction and be 0.01%～0.1% solder powder; Two, solder powder and scaling powder are mixed the back according to the mass ratio of 8 ﹕ 2 and be incubated 60s～80s melting under 170 ℃～180 ℃ condition, air cooling promptly gets Sn-58 Bi lead-free solder reinforced by carbon nano tube.
7. the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 6, the granularity that it is characterized in that the Sn-58Bi of eutectic described in step 1 alloyed powder is 25 μ m～75 μ m.
8. according to the preparation method of claim 6 or 7 described Sn-58 Bi lead-free solder reinforced by carbon nano tube, it is characterized in that scaling powder described in the step 2 is Flux55.
9. the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 8 is characterized in that described in the step 1 that the CNT mass fraction is 0.06% in the solder powder.
10. the preparation method of Sn-58 Bi lead-free solder reinforced by carbon nano tube according to claim 8 is characterized in that described in the step 1 that the CNT mass fraction is 0.03% in the solder powder.
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| CN102240866A (en) * | 2011-05-19 | 2011-11-16 | 哈尔滨工业大学 | Aluminum borate crystal whisker reinforced low-temperature unleaded composite soldering paste and preparation method thereof |
| CN103386559A (en) * | 2013-07-25 | 2013-11-13 | 常熟理工学院 | SnBi system low-temperature lead-free braze paste containing nanometer graphite |
| CN104416296A (en) * | 2013-09-03 | 2015-03-18 | 天津大学 | Method and application for improving electromigration resistance of interconnection welding spots of welding fluxes |
| CN106363315A (en) * | 2016-10-26 | 2017-02-01 | 亿铖达焊锡制造（昆山）有限公司 | Tinned carbon nanomaterial reinforced compound solder alloy and solder paste thereof |
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| CN102240866B (en) * | 2011-05-19 | 2013-03-27 | 哈尔滨工业大学 | Aluminum borate crystal whisker reinforced low-temperature unleaded composite soldering paste and preparation method thereof |
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| CN106363315A (en) * | 2016-10-26 | 2017-02-01 | 亿铖达焊锡制造（昆山）有限公司 | Tinned carbon nanomaterial reinforced compound solder alloy and solder paste thereof |
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| CN109609805A (en) * | 2018-12-18 | 2019-04-12 | 河南科技大学 | A kind of preparation process of c-based nanomaterial enhancing low melting point composite material |
| CN113492277A (en) * | 2020-03-19 | 2021-10-12 | 江苏奥匠新材料科技有限公司 | Low-temperature tin paste material with metal coating and carbon nanotube reinforcement and preparation method thereof |
| CN111872600A (en) * | 2020-07-08 | 2020-11-03 | 中国矿业大学 | MOFs carbonized product, preparation method and application in lead-free solder modification |
| CN113714677A (en) * | 2021-08-30 | 2021-11-30 | 江苏师范大学 | Sn-based brazing filler metal capable of realizing high-strength interconnection of CSP (chip scale package) devices |
| CN113714677B (en) * | 2021-08-30 | 2023-03-14 | 江苏师范大学 | Sn-based brazing filler metal capable of realizing high-strength interconnection of CSP (chip Scale Package) devices |
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Application publication date: 20100901 |