CN105014254B - A kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof - Google Patents
A kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof Download PDFInfo
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- CN105014254B CN105014254B CN201510455511.7A CN201510455511A CN105014254B CN 105014254 B CN105014254 B CN 105014254B CN 201510455511 A CN201510455511 A CN 201510455511A CN 105014254 B CN105014254 B CN 105014254B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/264—Bi as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Mechanical Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a kind of photovoltaic welding belt corrosion-resistant solder and preparation method thereof, the solder contains each component of following percentage by weight：55~60% Bi, 0~0.01% Sb, 0~0.0005% Al, 0~0.0005% Zn, surplus is tin；It the described method comprises the following steps：Appropriate tin and bismuth are mixed and heated to 280 300 DEG C, blend melt is obtained；Add appropriate bismuth chloride and cover the blend melt surface, it is then warm and be cooled to less than 180 DEG C after stirring 15 20 minutes, obtain fusion welding；Finally the fusion welding is filtered by porous carbon, then the fusion welding after filtering is cast, is produced；The solder of the present invention is by controlling key component Bi content, and fusing point is close to 139 DEG C after measured, and the solid liquid phase temperature difference is only 12 DEG C or so, it is possible to prevente effectively from segregation phenomena in the faster welding procedure of the cooldown rates such as immersed solder；And control the low content of impurity so that not only fusing point is low for the solder of preparation, and its corrosion resistance is also very strong.
Description
Technical field
The present invention relates to a kind of solder and preparation method thereof, and in particular to a kind of photovoltaic welding belt with corrosion-resistant solder and
Its preparation method.
Background technology
Photovoltaic welding belt is the key raw material of photovoltaic module production, plays conducting connection between cell piece, it can
The life-span of photovoltaic module is largely determined by property.
At present, because lead-free solder exists substantially in terms of the reliabilities such as corrosion resistance, anti-fatigue performance with solder containing pb
Performance difference, cause the unleaded application of photovoltaic module to be extremely restricted.Meanwhile, the welding usability of material is determined again
The efficiency and yield rate of component production, therefore it is required that reduction welding temperature, this fusing point to solder proposes new requirement.
Chinese patent (application number 201210494897.9) proposes a kind of low melting point lead-free solder alloy, contains Bi：
10%~30%, Ag：2.2%~3.0%, In：0.5%~1.0%, P：0.004%~0.008%, remaining is tin.But solder
Fusing point at 170 DEG C~200 DEG C or so, therefore appoint can not meet low-temperature welding requirement.Chinese patent (application number
201310345021.2) one kind series high strength lead-free low-temperature solders of Sn-Bi containing cobalt are disclosed, containing 54%~58% Bi,
0.5%~4.0% Ag, 0.1~1.0% Cu, 0.005%~0.08% Co, 0.002%~0.1% P and surplus are
Sn.The patent improves alloys wet power and intensity by elements such as Co, Ag, but is not directed to the corrosion resistance of material.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of photovoltaic welding belt with corrosion-resistant solder and
Its preparation method, so as to reach raising photovoltaic welding belt solder-coated layer surface corrosion resistant purpose while reducing fusing point.
To reach above-mentioned purpose, technical scheme is as follows：
On the one hand, the present invention provides a kind of corrosion-resistant solder of photovoltaic welding belt, and the solder contains following weight hundred
Divide each component of ratio：55~60% Bi, 0~0.01% Sb, 0~0.0005% Al, 0~0.0005% Zn, surplus
For tin.
The corrosion-resistant solder of photovoltaic welding belt of the present invention, by controlling the content of key component Bi (bismuth), after measured
Fusing point is close to 139 DEG C, and the solid liquid phase temperature difference is only 12 DEG C or so, can be effective in the faster welding procedure of the cooldown rates such as immersed solder
Avoid segregation phenomena；And control impurity Sb, Al and Zn low content so that not only fusing point is low for solder, and its corrosion resistance
Also it is very strong.
On the basis of above-mentioned technical proposal, the present invention can also make following improvement：
As preferred scheme, the weight percent content of the Bi is：59~60%.
Using above-mentioned preferred scheme, due to the cold characteristic risen of the pyrocondensation of bismuth element, determined through experiment when Bi contents are slightly higher
Contribute to improve photovoltaic welding belt surface local contraction phenomenon when eutectic composition (i.e. 59%~60%), improve surface smoothness
And further improve its decay resistance.
As preferred scheme, the weight percent content of the Sb is：0~0.003%.
The present invention photovoltaic welding belt can be realized with corrosion-resistant solder by a variety of methods, for example can be by following
Preparation method is realized.
On the other hand, the present invention also provides a kind of preparation method of photovoltaic welding belt of the invention with corrosion-resistant solder,
It the described method comprises the following steps：
1) appropriate tin and bismuth are mixed and heated to 280-300 DEG C, obtain blend melt；
2) add appropriate bismuth chloride and cover the blend melt surface, it is then warm and stir drop after 15-20 minute
Temperature obtains fusion welding to less than 180 DEG C；
3) finally the fusion welding is filtered by porous carbon, then the fusion welding after filtering is cast, produced.
The photovoltaic welding belt of the present invention preparation method of corrosion-resistant solder, during by controlling temperature and concrete operations
Between, BiCl 2 (bismuth chloride) is heated to the antimony in the replaceable solder of molten state, the high-melting-point chloride of formation, the porous carbon of use
The adsorbable tiny antimony chloride product of filtering material, can be efficiently separated through filtering, can be by the antimony content control in the solder of preparation
The ratio of system is relatively low, for example, can be controlled in below 100ppm, so as to obtain corrosion-resistant good eutectic solder alloy.
On the basis of above-mentioned technical proposal, the present invention can also make following improvement：
As preferred scheme, in step 3) in, after the fusion welding is filtered by porous carbon, also including with
Lower step：The fusion welding temperature is reduced to 150-155 DEG C, carbon monoxide is passed through fusion welding bottom and 30- is kept
40 minutes aluminum and zincs with reduction-oxidation, finally remove the slag system for floating on the fusion welding surface.
Using above-mentioned preferred scheme, by controlling specific temperature and recovery time in technique, aluminum and zinc is easily generated
Oxide, but be difficult to separate with solder compositions, after Carbon monoxide reduction, aluminium, zinc and gas form the foamed slag mixed more,
It is easy to separate and removes, can be relatively low by the ratio of the aluminum and zinc content control in the solder of preparation, below 5ppm is for example can be controlled in, from
And obtain corrosion-resistant good eutectic solder alloy.
As preferred scheme, the 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 the blend melt and bismuth chloride is 20: 1.
As preferred scheme, in step 3) in, the fusion welding is passed through into porous carbon filter 23-8 times.
As preferred scheme, in step 3) in, the fusion welding is imported into the graphite covered with porous carbon filter layer
Filtered in crucible.
Brief description of the drawings
Fig. 1 a are the fusing point test chart of solder prepared by the embodiment of the present invention 1；
Fig. 1 b are the fusing point test chart of solder prepared by the embodiment of the present invention 2；
Fig. 1 c are the fusing point test chart of solder prepared by the embodiment of the present invention 5；
Fig. 1 d are the fusing point test chart of solder prepared by comparative example 1 of the present invention；
Fig. 2 a are the Electronic Speculum result figure of solder made from embodiments of the invention 1；
Fig. 2 b are the Electronic Speculum result figure of solder made from embodiments of the invention 2；
Fig. 3 a are the corrosion-resistant result that welding surface after welding is made in solder prepared by comparative example 1 of the present invention；
Fig. 3 b are the corrosion-resistant result that welding surface after welding is made in solder prepared by the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail below by specific embodiment, but is not so limited the scope of the present invention.
Unless specifically stated otherwise, reagent used in following examples can be commercially available from regular channel.
Embodiment 1
Appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 300 DEG C of mixing first during melting molten
Body, then adds bismuth chloride powder covering blend melt surface (blend melt quality is 20: 1 with bismuth chloride mass ratio) warm
And it is cooled to 170 DEG C of acquisition fusion weldings after stirring 15 minutes, then fusion welding poured into covering porous carbon filter layer (thickness is
2 millimeters) graphite crucible, and by the filter 23 time repeatedly of the melt in graphite crucible.Fusion welding reduces temperature extremely after filtering
150 DEG C, it is passed through carbon monoxide from solder bottom and is kept for 30 minutes, finally the slag system for floating on bath surface is removed and cast, i.e.,
Obtain finished product.Through spark direct reading spectrometry and chemical method analysis (referring to：Standard GB/T/T 10574.1~13《Tin-lead solder chemistry
Analysis method》), solder bi content prepared by the technique is mass percent 58%, and remaining is impurity element and tin, impurity element
Middle content antimony (Sb) is that 98ppm, aluminium are that 4.9ppm, zinc are 4.7ppm.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, as a result as shown in Figure 1a, the solder melt point is approached
139 DEG C, the solid liquid phase temperature difference is only 11 DEG C or so.
And welding is made in the solder for preparing the embodiment.
Embodiment 2
Appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 280 DEG C of mixing first during melting molten
Body, then addition bismuth chloride powder covering bath surface (blend melt quality is 20: 1 with bismuth chloride mass ratio) is warm and stirs
Mix and 170 DEG C of fusion weldings are cooled to after 20 minutes, then fusion welding is poured into covering porous carbon filter layer (thickness is 2 millimeters)
Graphite crucible, and the melt in graphite crucible is filtered 5 times repeatedly.Fusion welding reduces temperature to 150 DEG C after filtering, from weldering
Material bottom is passed through carbon monoxide and kept for 30 minutes, finally removes the slag system for floating on bath surface and casts, gets product.Through fire
Flower direct reading spectrometry and chemical method analysis, solder bi content prepared by the technique is mass percent 59%, and remaining is impurity element
And tin；Impurity content antimony is that 78ppm, aluminium are that 4.3ppm, zinc are 4.2ppm in the solder.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, as a result as shown in Figure 1 b, the solder melt point is approached
139 DEG C, the solid liquid phase temperature difference is only 12 DEG C or so.
Embodiment 3
Appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 280 DEG C of mixing first during melting molten
Body, then adds chlorination bismuth meal warm to blend melt surface (blend melt quality is 20: 1 with bismuth chloride mass ratio) is covered
And it is cooled to 175 DEG C of acquisition fusion weldings after stirring 18 minutes, then fusion welding poured into covering porous carbon filter layer (thickness is
2 millimeters) graphite crucible, and the melt in graphite crucible is filtered 8 times repeatedly.Fusion welding reduces temperature extremely after filtering
150 DEG C, it is passed through carbon monoxide from solder bottom and is kept for 40 minutes, finally the slag system for floating on bath surface is removed and cast, i.e.,
Obtain finished product.Analyzed through spark direct reading spectrometry and chemical method, solder bi content prepared by the technique is mass percent 60%, remaining
For impurity element and tin；Impurity content antimony is that 66ppm, aluminium are that 3.5ppm, zinc are 3.4ppm in the solder.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, is as a result shown, the solder melt point close to 140 DEG C,
The solid liquid phase temperature difference is only 12 DEG C or so.
Embodiment 4
Appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 290 DEG C of mixing first during melting molten
Body, then adds chlorination bismuth meal warm to blend melt surface (solder melt quality is 20: 1 with bismuth chloride mass ratio) is covered
And it is cooled to 165 DEG C of acquisition fusion weldings after stirring 15 minutes, then fusion welding poured into covering porous carbon filter layer (thickness is
2 millimeters) graphite crucible, and the melt in graphite crucible is filtered 6 times repeatedly.Fusion welding reduces temperature extremely after filtering
152 DEG C, it is passed through carbon monoxide from solder bottom and is kept for 30 minutes, finally the slag system for floating on bath surface is removed and cast, i.e.,
Obtain finished product.Analyzed through spark direct reading spectrometry and chemical method, solder bi content prepared by the technique is mass percent 55%, remaining
For impurity element and tin.Impurity content antimony is that 73ppm, aluminium are that 4.0ppm, zinc are 3.6ppm in the solder.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, is as a result shown, the solder melt point close to 141 DEG C,
The solid liquid phase temperature difference is only 13 DEG C or so.
Embodiment 5
Appropriate pure tin (99.95%) and pure bismuth (99.95%) are mixed and heated to 300 DEG C of mixing first during melting molten
Body, then adds bismuth chloride powder covering blend melt surface (blend melt quality is 20: 1 with bismuth chloride mass ratio) warm
And it is cooled to 170 DEG C of acquisition fusion weldings after stirring 15 minutes, then fusion welding poured into covering porous carbon filter layer (thickness is
2 millimeters) graphite crucible, and by the filter 23 time repeatedly of the melt in graphite crucible.Fusion welding reduces temperature extremely after filtering
155 DEG C, it is passed through carbon monoxide from solder bottom and is kept for 35 minutes, finally the slag system for floating on bath surface is removed and cast, i.e.,
Obtain finished product.Analyzed through spark direct reading spectrometry and chemical method, solder bi content prepared by the technique is mass percent 56%, remaining
For impurity element and tin, impurity content antimony is that 98ppm, aluminium are that 4.9ppm, zinc are 4.7ppm.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, as a result as illustrated in figure 1 c, the solder melt point is approached
140 DEG C, the solid liquid phase temperature difference is only 12 DEG C or so.
And welding is made in the solder for preparing the embodiment.
Comparative example 1
The method for preparing solder is same as Example 1, different not add the step that BiCl2 remove antimony for blend melt
Suddenly, fusion welding does not add the step of Carbon monoxide reduction removes zinc and aluminium yet.Analyzed through spark direct reading spectrometry and chemical method, should
Solder bi content prepared by technique is mass percent 54%, and remaining is impurity element and tin.Impurity content in the solder
Antimony is that 177ppm, aluminium are that 8.9ppm, zinc are 8.0ppm.
And welding is made in the solder for preparing the embodiment.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, as a result as shown in Figure 1 d, the solder melt point is approached
142 DEG C, the solid liquid phase temperature difference is 15 DEG C or so, and its melting range is relatively long.
Comparative example 2
The method for preparing solder is same as Example 1, and different is：Chlorination bismuth meal is added into blend melt, covering mixing
Bath surface (solder melt quality with bismuth chloride mass ratio be 20: 1) is warm and is cooled to 190 DEG C of acquisitions after stirring 10 minutes
Fusion welding.
Analyzed through spark direct reading spectrometry and chemical method, solder bi content prepared by the technique is mass percent 54%, its
Remaining is impurity element and tin.Impurity content antimony is that 114ppm, aluminium are that 7.9ppm, zinc are 7.3ppm in the solder.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, is as a result shown, the solder melt point close to 142 DEG C,
The solid liquid phase temperature difference is 15 DEG C or so, and its melting range is relatively long.
Comparative example 3
The method for preparing solder is same as Example 1, and different is：Fusion welding reduces temperature to 148 DEG C after filtering,
Carbon monoxide is passed through from solder bottom and is kept for 20 minutes, and the slag system for floating on bath surface is finally removed into casting and got product.
Analyzed through spark direct reading spectrometry and chemical method, solder bi content prepared by the technique is mass percent 54%, its
Remaining is impurity element and tin.Impurity content antimony is that 82ppm, aluminium are that 6.1ppm, zinc are 5.8ppm in the solder.
Then the melting point curve of the solder is tested through differential scanning calorimetric gauge, is as a result shown, the solder melt point close to 142 DEG C,
The solid liquid phase temperature difference is only 15 DEG C or so, and its melting range is relatively long.
Solder made from embodiment 1 and embodiment 2 is observed under a scanning electron microscope, as a result such as Fig. 2 a and Fig. 2 b institutes
Show, as can be seen from the figure because bi content is higher, its constriction zone is small, welding surface more even uniform illustrates when Bi contains
Amount contributes to improve photovoltaic welding belt surface local contraction phenomenon when being slightly above eutectic composition (i.e. 59%-60%), improves surface
Finish simultaneously further improves its decay resistance.
Welding prepared by welding and embodiment 1 prepared by comparative example 1 is by salt air corrosion 48 hours, in scanning electron
The surface of micro- Microscopic observation welding, as a result as best shown in figures 3 a and 3b, as can be seen from the figure after salt air corrosion, in Fig. 3 a
The local corrosion (white product) for being centered around solidification shrinkage region is found that, and does not find similar corrosion product in Fig. 3 b, i.e.,
The corrosion resistance of welding is substantially better than welding prepared by non-purified technique made from the preparation method of the present invention；And due to right
The content of bismuth metal is relatively low in ratio, and the fusing point of its solder being made is of a relatively high.
Above example illustrates, solder of the invention is by controlling key component Bi content, and fusing point is close to 139 after measured
DEG C, the solid liquid phase temperature difference is only 12 DEG C or so, it is possible to prevente effectively from segregation is existing in the faster welding procedure of the cooldown rates such as immersed solder
As；And control impurity Sb, Al and Zn low content so that not only fusing point is low for the solder of preparation, and its corrosion resistance is also very
By force；And the content of solder metal bismuth made from comparative example is relatively low, the fusing point of its solder being made is of a relatively high, and due to not having
Operated by the process of the present invention, its impurity content is substantially high, and corrosion resistance is poor.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (8)
1. a kind of photovoltaic welding belt preparation method of corrosion-resistant solder, the solder contains each group of following percentage by weight
Point：55~60% Bi, 0~0.01% Sb, 0~0.0005% Al, 0~0.0005% Zn, surplus is tin；Described
Photovoltaic welding belt uses following preparation method with corrosion-resistant solder, the described method comprises the following steps：
1) appropriate tin and bismuth are mixed and heated to 280-300 DEG C, obtain blend melt；
2) add appropriate bismuth chloride and cover the blend melt surface, it is then warm and be cooled to after stirring 15-20 minutes
Less than 180 DEG C, obtain fusion welding；
3) finally the fusion welding is filtered by porous carbon, the fusion welding temperature is reduced to 150-155 DEG C, by one
Carbonoxide is passed through fusion welding bottom and keeps the 30-40 minutes aluminum and zincs with reduction-oxidation, will finally float on the fusion weld
Expect that the slag system on surface is removed, then fusion welding is cast, produce.
2. the photovoltaic welding belt according to claim 1 preparation method of corrosion-resistant solder, it is characterised in that the Bi
Weight percent content be：59~60%.
3. the photovoltaic welding belt according to claim 1 preparation method of corrosion-resistant solder, it is characterised in that the Sb
Weight percent content be：0~0.003%.
4. the photovoltaic welding belt according to claim 1 preparation method of corrosion-resistant solder, it is characterised in that in step
3) in, the fusion welding temperature is reduced to 150 DEG C.
5. the photovoltaic welding belt according to any one of claim 1 to 4 preparation method of corrosion-resistant solder, its feature
It is, in step 1) in, appropriate tin and bismuth are mixed and heated to 300 DEG C.
6. the photovoltaic welding belt according to any one of claim 1 to 4 preparation method of corrosion-resistant solder, its feature
It is, in step 2) in, stir 15 minutes.
7. the photovoltaic welding belt according to any one of claim 1 to 4 preparation method of corrosion-resistant solder, in step
2) in, the mass ratio of the blend melt and bismuth chloride is 20: 1.
8. the photovoltaic welding belt according to any one of claim 1 to 4 preparation method of corrosion-resistant solder, its feature
It is, in step 3) in, the fusion welding is imported in the graphite crucible covered with porous carbon filter layer and filtered.
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| CN109093282A (en) * | 2018-09-30 | 2018-12-28 | 苏州宇邦新型材料股份有限公司 | A kind of corrosion-resistant solder of Sn-Pb-Bi and preparation method thereof of the photovoltaic welding belt containing Al |
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| TWI646203B (en) * | 2016-07-15 | 2019-01-01 | 日商Ｊｘ金屬股份有限公司 | Solder alloy |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109093282A (en) * | 2018-09-30 | 2018-12-28 | 苏州宇邦新型材料股份有限公司 | A kind of corrosion-resistant solder of Sn-Pb-Bi and preparation method thereof of the photovoltaic welding belt containing Al |
| CN109093282B (en) * | 2018-09-30 | 2021-08-03 | 苏州宇邦新型材料股份有限公司 | Sn-Pb-Bi corrosion-resistant solder containing Al for photovoltaic solder strip and preparation method thereof |
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| CN105014254A (en) | 2015-11-04 |
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