CN105014254A - Corrosion-resistant low-temperature solder for photovoltaic solder strip and preparation method of corrosion-resistant low-temperature solder - Google Patents

Corrosion-resistant low-temperature solder for photovoltaic solder strip and preparation method of corrosion-resistant low-temperature solder Download PDF

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Publication number
CN105014254A
CN105014254A CN201510455511.7A CN201510455511A CN105014254A CN 105014254 A CN105014254 A CN 105014254A CN 201510455511 A CN201510455511 A CN 201510455511A CN 105014254 A CN105014254 A CN 105014254A
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solder
corrosion
preparation
photovoltaic
welding
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CN105014254B (en
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肖锋
周健
陈旭
朱骄峰
李赛鹏
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SUZHOU YOURBEST NEW-TYPE MATERIALS Co Ltd
Southeast University
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SUZHOU YOURBEST NEW-TYPE MATERIALS Co Ltd
Southeast University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/26Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/264Bi as the principal constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40Making wire or rods for soldering or welding

Abstract

The invention discloses corrosion-resistant low-temperature solder for a photovoltaic solder strip and a preparation method of the corrosion-resistant low-temperature solder. The solder comprises, by weight, 55%-60% of Bi, 0-0.01% of Sb, 0-0.0005% of Al, 0-0.0005% of Zn and the balance tin. The method comprises the following steps that a proper amount of the tin and bismuth is heated to 280 DEG C to 300 DEG C, and mixed melt is obtained; a proper amount of bismuth chloride is added to cover the surface of the mixed melt, then heat preservation is carried out, temperature is reduced to below 180 DEG C after stirring of 15-20 minutes, and molten solder is obtained; and finally the molten solder is filtered through porous carbon, the filtered molten solder is cast, and the corrosion-resistant low-temperature solder is obtained. According to the solder, the content of the key component Bi is controlled, it is measured that the melting point is close to 139 DEG C, the temperature difference of a solid phase and a liquid phase is only about 12 DEG C, and the phenomenon of segregation can be effectively avoided in dip soldering and other welding processes with the high cooling rate; the content of impurities is controlled to be low, so that the melting point of the prepared solder is low, and the corrosion resistance of the prepared solder is high.

Description

A kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof
Technical field
The present invention relates to a kind of solder and preparation method thereof, be specifically related to a kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof.
Background technology
Photovoltaic welding belt is the key raw material that photovoltaic module is produced, and between cell piece, play conducting connect, its reliability determines the life-span of photovoltaic module to a great extent.
At present, because lead-free solder exists obvious performance difference with solder containing pb in the reliability such as corrosion resistance, anti-fatigue performance, the unleaded application of photovoltaic module is caused to be extremely restricted.Meanwhile, the welding usability of material determines again efficiency and the yield rate of assembly production, and therefore require to reduce welding temperature, this proposes new requirement to the fusing point of solder.
Chinese patent (application number 201210494897.9) proposes a kind of low melting point lead-free solder alloy, and containing Bi:10% ~ 30%, Ag:2.2% ~ 3.0%, In:0.5% ~ 1.0%, P:0.004% ~ 0.008%, all the other are tin.But the fusing point of solder, at 170 DEG C ~ about 200 DEG C, is therefore appointed and can not be met low-temperature welding requirement.Chinese patent (application number 201310345021.2) discloses a kind of containing cobalt Sn-Bi series high strength lead-free low-temperature solder, the Bi containing 54% ~ 58%, the Ag of 0.5% ~ 4.0%, 0.1 ~ 1.0% Cu, the Co of 0.005% ~ 0.08%, the P of 0.002% ~ 0.1% and surplus be Sn.This patent improves alloys wet power and intensity by elements such as Co, Ag, but does not relate to the corrosion resistance of material.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof, thus while reducing fusing point, reach the object improving the erosion of photovoltaic welding belt solder-coated layer surface corrosion-resistant.
For achieving the above object, technical scheme of the present invention is as follows:
On the one hand, the invention provides the corrosion-resistant solder of a kind of photovoltaic welding belt, described solder contains each component of following percentage by weight: the Bi of 55 ~ 60%, the Sb of 0 ~ 0.01%, the Al of 0 ~ 0.0005%, the Zn of 0 ~ 0.0005%, and surplus is tin.
The corrosion-resistant solder of photovoltaic welding belt of the present invention, by controlling the content of key component Bi (bismuth), fusing point is close to 139 DEG C after measured, and the solid liquid phase temperature difference is only about 12 DEG C, can effectively avoid segregation phenomena in the cooldown rates such as immersed solder faster welding procedure; And control the low content of impurity Sb, Al and Zn, not only fusing point is low to make solder, and its corrosion resistance is also very strong.
On the basis of technique scheme, the present invention also can make following improvement:
As preferred scheme, the weight percent content of described Bi is: 59 ~ 60%.
Adopt above-mentioned preferred scheme, the cold characteristic risen of pyrocondensation due to bismuth element, improving photovoltaic welding belt surface local contraction phenomenon when Bi content a little more than contributing to time eutectic composition (namely 59% ~ 60%) through test determination, improving surface smoothness and improving its decay resistance further.
As preferred scheme, the weight percent content of described Sb is: 0 ~ 0.003%.
The corrosion-resistant solder of photovoltaic welding belt of the present invention realizes by multiple method, such as, realize by following preparation method.
On the other hand, the present invention also provides a kind of photovoltaic welding belt of the present invention preparation method of corrosion-resistant solder, said method comprising the steps of:
1) appropriate tin and bismuth are mixed and heated to 280-300 DEG C, obtain blend melt;
2) add appropriate bismuth chloride again and cover described blend melt surface, then after being incubated and stir 15-20 minute, be cooled to less than 180 DEG C, obtain fusion welding;
3) finally described fusion welding is filtered by porous carbon, then the fusion welding after filtering is cast, to obtain final product.
The photovoltaic welding belt of the present invention preparation method of corrosion-resistant solder, by control temperature and concrete operations time, BiCl 2(bismuth chloride) is heated to the antimony in the replaceable solder of molten state, the high-melting-point chloride formed, the adsorbable tiny antimony chloride product of porous carbon filtering material adopted, can effectively be separated after filtration, what the antimony content in the solder of preparation can be controlled is lower, such as can be controlled in below 100ppm, thus obtain corrosion-resistant good eutectic solder alloy.
On the basis of technique scheme, the present invention also can make following improvement:
As preferred scheme, in step 3) in, after described fusion welding is filtered by porous carbon, further comprising the steps of: described fusion welding temperature is reduced to 150-155 DEG C, being passed into by carbon monoxide bottom fusion welding and to keep 30-40 minute with the aluminum and zinc of reduction-oxidation, the slag system that finally will float on described fusion welding surface is removed.
Adopt above-mentioned preferred scheme, by temperature concrete in Controlling Technology and recovery time, aluminum and zinc is easy to generate oxide, but be difficult to be separated with solder compositions, after Carbon monoxide reduction, aluminium, zinc and gas form the heterogeneous foamed slag mixed, be convenient to be separated and remove, what the aluminum and zinc content in the solder of preparation can be controlled is lower, such as, can be controlled in below 5ppm, thus obtain corrosion-resistant good eutectic solder alloy.
As preferred scheme, described fusion welding temperature is reduced to 150 DEG C.
As preferred scheme, in step 1) in, appropriate tin and bismuth are mixed and heated to 300 DEG C.
As preferred scheme, in step 2) in, stir 15 minutes.
As preferred scheme, in step 2) in, the mass ratio of described blend melt and bismuth chloride is 20: 1.
As preferred scheme, in step 3) in, described fusion welding is passed through porous carbon filter 23-8 times.
As preferred scheme, in step 3) in, described fusion welding is imported to be coated with in the graphite crucible of porous carbon filter course and filters.
Accompanying drawing explanation
Fig. 1 a is the fusing point resolution chart of solder prepared by the embodiment of the present invention 1;
Fig. 1 b is the fusing point resolution chart of solder prepared by the embodiment of the present invention 2;
Fig. 1 c is the fusing point resolution chart of solder prepared by the embodiment of the present invention 5;
Fig. 1 d is the fusing point resolution chart of the solder of comparative example 1 of the present invention preparation;
Fig. 2 a is the Electronic Speculum result figure of the solder that embodiments of the invention 1 obtain;
Fig. 2 b is the Electronic Speculum result figure of the solder that embodiments of the invention 2 obtain;
Fig. 3 a is the corrosion-resistant result that welding surface after welding made by the solder of comparative example 1 of the present invention preparation;
Fig. 3 b is the corrosion-resistant result that welding surface after welding made by solder prepared by the embodiment of the present invention 1.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, but does not therefore limit the scope of the invention.
Unless specifically stated otherwise, reagent used in following examples all can be commercially available from regular channel.
Embodiment 1
First appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 300 DEG C of blend melt during melting, then add bismuth chloride powder to cover blend melt surface (blend melt quality and bismuth chloride mass ratio are 20: 1) and after being incubated and stir 15 minutes, being cooled to 170 DEG C obtaining fusion welding, again fusion welding is poured into the graphite crucible covering porous carbon filter course (thickness is 2 millimeters), and by the filter 23 repeatedly of the melt in graphite crucible.After filtering, fusion welding reduces temperature to 150 DEG C, passes into carbon monoxide and keep 30 minutes bottom solder, finally the slag system floating on bath surface is removed casting, gets product.Through spark direct reading spectrometry and chemical method analysis (see: standard GB/T/T 10574.1 ~ 13 " tin-lead solder chemical analysis method "), solder bi content prepared by this technique is mass percent 58%, all the other are impurity element and tin, and in impurity element, content antimony (Sb) is 98ppm, aluminium is 4.9ppm, zinc is 4.7ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, as shown in Figure 1a, this solder melt point is close to 139 DEG C, and the solid liquid phase temperature difference is only about 11 DEG C for result.
And solder prepared by this embodiment is made welding.
Embodiment 2
First appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 280 DEG C of blend melt during melting, then add bismuth chloride powder covering bath surface (blend melt quality and bismuth chloride mass ratio are 20: 1) and be cooled to 170 DEG C of fusion weldings after being incubated and stir 20 minutes, again fusion welding is poured into the graphite crucible covering porous carbon filter course (thickness is 2 millimeters), and the melt in graphite crucible is filtered 5 times repeatedly.After filtering, fusion welding reduces temperature to 150 DEG C, passes into carbon monoxide and keep 30 minutes bottom solder, finally the slag system floating on bath surface is removed casting, gets product.Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 59%, and all the other are impurity element and tin; In this solder, impurity content antimony is 78ppm, aluminium is 4.3ppm, zinc is 4.2ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, result as shown in Figure 1 b, this solder melt point is close to 139 DEG C, and the solid liquid phase temperature difference is only about 12 DEG C.
Embodiment 3
First appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 280 DEG C of blend melt during melting, then add chlorination bismuth meal after being incubated and stir 18 minutes, being cooled to 175 DEG C obtaining fusion welding to covering blend melt surface (blend melt quality and bismuth chloride mass ratio are 20: 1), again fusion welding is poured into the graphite crucible covering porous carbon filter course (thickness is 2 millimeters), and the melt in graphite crucible is filtered 8 times repeatedly.After filtering, fusion welding reduces temperature to 150 DEG C, passes into carbon monoxide and keep 40 minutes bottom solder, finally the slag system floating on bath surface is removed casting, gets product.Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 60%, and all the other are impurity element and tin; In this solder, impurity content antimony is 66ppm, aluminium is 3.5ppm, zinc is 3.4ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, result shows, this solder melt point is close to 140 DEG C, and the solid liquid phase temperature difference is only about 12 DEG C.
Embodiment 4
First appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 290 DEG C of blend melt during melting, then add chlorination bismuth meal after being incubated and stir 15 minutes, being cooled to 165 DEG C obtaining fusion welding to covering blend melt surface (solder melt quality and bismuth chloride mass ratio are 20: 1), again fusion welding is poured into the graphite crucible covering porous carbon filter course (thickness is 2 millimeters), and the melt in graphite crucible is filtered 6 times repeatedly.After filtering, fusion welding reduces temperature to 152 DEG C, passes into carbon monoxide and keep 30 minutes bottom solder, finally the slag system floating on bath surface is removed casting, gets product.Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 55%, and all the other are impurity element and tin.In this solder, impurity content antimony is 73ppm, aluminium is 4.0ppm, zinc is 3.6ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, result shows, this solder melt point is close to 141 DEG C, and the solid liquid phase temperature difference is only about 13 DEG C.
Embodiment 5
First appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 300 DEG C of blend melt during melting, then add bismuth chloride powder to cover blend melt surface (blend melt quality and bismuth chloride mass ratio are 20: 1) and after being incubated and stir 15 minutes, being cooled to 170 DEG C obtaining fusion welding, again fusion welding is poured into the graphite crucible covering porous carbon filter course (thickness is 2 millimeters), and by the filter 23 repeatedly of the melt in graphite crucible.After filtering, fusion welding reduces temperature to 155 DEG C, passes into carbon monoxide and keep 35 minutes bottom solder, finally the slag system floating on bath surface is removed casting, gets product.Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 56%, and all the other are impurity element and tin, and impurity content antimony is 98ppm, aluminium is 4.9ppm, zinc is 4.7ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, as illustrated in figure 1 c, this solder melt point is close to 140 DEG C, and the solid liquid phase temperature difference is only about 12 DEG C for result.
And solder prepared by this embodiment is made welding.
Comparative example 1
The method preparing solder is identical with embodiment 1, and different is the step that blend melt does not add that BiCl2 carries out removing antimony, and fusion welding does not add the step that Carbon monoxide reduction removes zinc and aluminium yet.Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 54%, and all the other are impurity element and tin.In this solder, impurity content antimony is 177ppm, aluminium is 8.9ppm, zinc is 8.0ppm.
And solder prepared by this embodiment is made welding.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, as shown in Figure 1 d, this solder melt point is close to 142 DEG C, and the solid liquid phase temperature difference is about 15 DEG C, and its melting range is relatively long for result.
Comparative example 2
The method preparing solder is identical with embodiment 1, different is: chlorination bismuth meal is added blend melt, and covering blend melt surface (solder melt quality and bismuth chloride mass ratio are 20: 1) is cooled to 190 DEG C and obtains fusion welding after being incubated and stir 10 minutes.
Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 54%, and all the other are impurity element and tin.In this solder, impurity content antimony is 114ppm, aluminium is 7.9ppm, zinc is 7.3ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, result shows, this solder melt point is close to 142 DEG C, and the solid liquid phase temperature difference is about 15 DEG C, and its melting range is relatively long.
Comparative example 3
The method preparing solder is identical with embodiment 1, and different is: after filtering, fusion welding reduces temperature to 148 DEG C, passes into carbon monoxide and keep 20 minutes bottom solder, finally the slag system floating on bath surface is removed casting and gets product.
Through spark direct reading spectrometry and chemical method analysis, solder bi content prepared by this technique is mass percent 54%, and all the other are impurity element and tin.In this solder, impurity content antimony is 82ppm, aluminium is 6.1ppm, zinc is 5.8ppm.
Then test the melting point curve of this solder through differential scanning calorimetric gauge, result shows, this solder melt point is close to 142 DEG C, and the solid liquid phase temperature difference is only about 15 DEG C, and its melting range is relatively long.
Experimental example 1
Observe embodiment 1 and the obtained solder of embodiment 2 under a scanning electron microscope, result as shown in Figure 2 a and 2 b, as can be seen from the figure because bi content is higher, its constriction zone is little, welding surface even uniform more, illustrating when Bi content improves photovoltaic welding belt surface local contraction phenomenon a little more than contributing to time eutectic composition (i.e. 59%-60%), improving surface smoothness and improving its decay resistance further.
Experimental example 2
Welding prepared by the welding prepare comparative example 1 and embodiment 1 is all by salt air corrosion 48 hours, observe the surface of welding under a scanning electron microscope, result as best shown in figures 3 a and 3b, as can be seen from the figure after salt air corrosion, the local corrosion (white product) being centered around solidification shrinkage region has been found in Fig. 3 a, and in Fig. 3 b, not finding similar corrosion product, the corrosion resistance of welding that namely preparation method of the present invention obtains obviously is better than welding prepared by non-process for purifying; And because in comparative example, the content of bismuth metal is lower, the fusing point of its solder made is relatively high.
Above embodiment illustrates, solder of the present invention is by controlling the content of key component Bi, and fusing point is close to 139 DEG C after measured, and the solid liquid phase temperature difference is only about 12 DEG C, can effectively avoid segregation phenomena in the cooldown rates such as immersed solder faster welding procedure; And control the low content of impurity Sb, Al and Zn, not only fusing point is low to make the solder prepared, and its corrosion resistance is also very strong; And the content of the solder metal bismuth that comparative example obtains is lower, the fusing point of its solder made is relatively high, and owing to not operating by process of the present invention, its impurity content is obviously high, and corrosion resistance is poor.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.

Claims (10)

1. the corrosion-resistant solder of photovoltaic welding belt, described solder contains each component of following percentage by weight: the Bi of 55 ~ 60%, the Sb of 0 ~ 0.01%, the Al of 0 ~ 0.0005%, the Zn of 0 ~ 0.0005%, and surplus is tin.
2. the corrosion-resistant solder of photovoltaic welding belt according to claim 1, is characterized in that, the weight percent content of described Bi is: 59 ~ 60%.
3. the corrosion-resistant solder of photovoltaic welding belt according to claim 1, is characterized in that, the weight percent content of described Sb is: 0 ~ 0.003%.
4. the photovoltaic welding belt according to any one of claim 1 to 3 preparation method of corrosion-resistant solder, said method comprising the steps of:
1) appropriate tin and bismuth are mixed and heated to 280-300 DEG C, obtain blend melt;
2) add appropriate bismuth chloride again and cover described blend melt surface, then after being incubated and stir 15-20 minute, be cooled to less than 180 DEG C, obtain fusion welding;
3) finally described fusion welding is filtered by porous carbon, then the fusion welding after filtering is cast, to obtain final product.
5. the photovoltaic welding belt according to claim 4 preparation method of corrosion-resistant solder, it is characterized in that, in step 3) in, after described fusion welding is filtered by porous carbon, further comprising the steps of: described fusion welding temperature is reduced to 150-155 DEG C, being passed into by carbon monoxide bottom fusion welding and to keep 30-40 minute with the aluminum and zinc of reduction-oxidation, the slag system that finally will float on described fusion welding surface is removed.
6. the photovoltaic welding belt according to claim 5 preparation method of corrosion-resistant solder, is characterized in that, described fusion welding temperature is reduced to 150 DEG C.
7. the preparation method of corrosion-resistant solder of the photovoltaic welding belt according to any one of claim 4 to 6, is characterized in that, in step 1) in, appropriate tin and bismuth are mixed and heated to 300 DEG C.
8. the preparation method of corrosion-resistant solder of the photovoltaic welding belt according to any one of claim 4 to 6, is characterized in that, in step 2) in, stir 15 minutes.
9. the preparation method of corrosion-resistant solder of the photovoltaic welding belt according to any one of claim 4 to 6, in step 2) in, the mass ratio of described blend melt and bismuth chloride is 20: 1.
10. the preparation method of corrosion-resistant solder of the photovoltaic welding belt according to any one of claim 4 to 6, is characterized in that, in step 3) in, described fusion welding is imported to be coated with in the graphite crucible of porous carbon filter course and filters.
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CN111250893A (en) * 2020-03-12 2020-06-09 南通欢腾机电科技有限公司 Lead-free solder, preparation method and application thereof, and metal terminal
CN113231757A (en) * 2021-06-22 2021-08-10 内蒙古玉桥合金材料制造有限公司 Tin-based soldering paste and preparation method thereof
CN114012303A (en) * 2021-10-28 2022-02-08 宁波佳明金属制品有限公司 Low-temperature solder and preparation method thereof

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