CN106119755A - A kind of antioxidation tin plating electrolyte based on indium gallium phosphorus - Google Patents
A kind of antioxidation tin plating electrolyte based on indium gallium phosphorus Download PDFInfo
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- CN106119755A CN106119755A CN201610789854.1A CN201610789854A CN106119755A CN 106119755 A CN106119755 A CN 106119755A CN 201610789854 A CN201610789854 A CN 201610789854A CN 106119755 A CN106119755 A CN 106119755A
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- tin plating
- phosphorus
- plating electrolyte
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/08—Tin or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
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- Chemical Kinetics & Catalysis (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention belongs to metal oxidation resistance resist technology field, specifically disclose a kind of antioxidation tin plating electrolyte, comprise following component: indium, gallium, phosphorus, stannum.Wherein, on the basis of the weight of described stannum, the percentage by weight of described indium is 0.005% 0.04%, and the percentage by weight of described gallium is 0.005% 0.06%, and the percentage by weight of described phosphorus is 0.01% 0.05%.The present invention adds indium, gallium, phosphorus in tin liquor, can effectively suppress the oxidation of tin plating electrolyte, reduces the generation of scruff, has significant effect for improving stannum product lumber recovery, raising hot tinning production rate etc.；The wettability of tin plating electrolyte is slightly promoted simultaneously, the fusing point of tin-plated product is slightly reduced, and do not affect other physical and mechanical properties of tin-plated product；The antioxidation tin plating electrolyte low cost of the present invention, does not change existing production technology, does not affect existing equipment regular maintenance and maintenance, meet environmental requirement, do not affect the working environment of Workplace.
Description
Technical field
The present invention relates to metal oxidation resistance resist technology field, be specifically related to a kind of antioxidation based on indium gallium phosphorus tin plating
Liquid, is mainly used in photovoltaic welding belt.
Background technology
Along with the fast development of electron trade, fusing point is low, good corrosion resistance is combined with metallic matrix because having for kamash alloy
Property the advantage such as good, be widely used in the field such as photovoltaic welding belt, Electronic Packaging.But, the liquid tin alloy pole under molten condition
Oxidizable formation scruff, block tin, wherein contain a large amount of unoxidized stannum, cause raw material to utilize insufficient, produces waste, increases
Production cost, also can affect the quality of product.Additionally, in the production process of photovoltaic welding belt, in stannum stove, the oxidation of ashbury metal is also
Aberration can be produced on welding surface, affect outward appearance, and easily form black speck during the transport and storage in later stage, cause producing
Product are scrapped.In order to ensure the reliability of welding, need to improve the antioxygenic property of kamash alloy.
The oxidation measure solving melt stannum at present mainly has melt cladding process, protective atmosphere method and melt modification method.Melt
Coverture in cladding process easily remains, and readily volatilized, the carbonization of being heated, smolders, pollutes environment, additionally, general coverture
For inorganic salts, easily production equipment is caused heavy corrosion, affect the production order.Atmosphere protection method processing equipment is huge, raw
Product cost is high.Melt modification rule only need to be on the premise of ensureing scolding tin self wettability, brazing property, by adding alloy
Element is to stannum melt modification, to improve its antioxygenic property, has that production operation is simple, input cost is low, not by external environment
The advantages such as impact.
But existing antioxidant is relatively costly on market, specific aim is relatively strong, and antioxidative effect is not satisfactory, and main
Will can bring the problem such as devil liquor recovery, environmental pollution based on organic solvent, the method added by inorganic elements improves stannum
The antioxygenic property of melt seldom has actually used case.
Summary of the invention
For problems of the prior art, it is an object of the invention to provide the base that a kind of low cost, the suitability are strong
In the antioxidation tin plating electrolyte of indium gallium phosphorus, its antioxygenic property is high, is effectively reduced the generation amount of scruff/block tin, improves the profit of stannum
By rate, it is mainly used in photovoltaic welding belt.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A kind of antioxidation tin plating electrolyte based on indium gallium phosphorus, it is characterised in that comprise following component: indium, gallium, phosphorus, stannum.
Preferably, on the basis of the weight of described stannum, the percentage by weight of described indium is 0.005%-0.04%, described gallium
Percentage by weight be 0.005%-0.06%, the percentage by weight of described phosphorus is 0.01%-0.05%.
Preferably, the percentage by weight of described indium is 0.01%-0.04%.
Preferably, the percentage by weight of described gallium is 0.01%-0.06%.
Preferably, the percentage by weight of described phosphorus is 0.02%-0.04%.
Owing to the industrial temperature of tin liquor is relatively low, when adding anti-oxidizing elements indium, gallium, phosphorus, these elements all can not be quick
Melt, and can not merge uniformly with tin liquor, accordingly, it would be desirable to be configured to the kamash alloy of certain content.
Preferably, described indium is tin plating with the form described antioxidation based on indium gallium phosphorus of fusing preparation of indium-stannum intermediate alloy
Liquid.
Preferably, described gallium is tin plating with the form described antioxidation based on indium gallium phosphorus of fusing preparation of gallium-stannum intermediate alloy
Liquid.
Preferably, described phosphorus is tin plating with the form described antioxidation based on indium gallium phosphorus of fusing preparation of phosphorus-stannum intermediate alloy
Liquid.
Preferably, in described indium-stannum intermediate alloy, the content of indium is the 5% of described indium-stannum intermediate alloy quality.
Preferably, in described gallium-stannum intermediate alloy, the content of gallium is the 5% of described gallium-stannum intermediate alloy quality.
Preferably, in described phosphorus-stannum intermediate alloy, the content of phosphorus is the 5% of described phosphorus-stannum intermediate alloy quality.
Compared with prior art, the invention have the benefit that
The present invention adds indium, gallium, phosphorus in tin liquor, can effectively suppress the oxidation of tin plating electrolyte, reduces the generation of scruff, for
Improve stannum product lumber recovery, raising hot tinning production rate etc. and also there is significant effect；Wettability to tin plating electrolyte simultaneously
Slightly promote, the fusing point of tin-plated product is slightly reduced, and do not affect other physical and mechanical properties of tin-plated product；The present invention
Antioxidation tin plating electrolyte low cost, do not change existing production technology, do not affect existing equipment regular maintenance and maintenance；Meet ring
Guaranteed request, does not affect the working environment of Workplace.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but those skilled in the art will
It will be appreciated that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the present invention.
The invention provides a kind of antioxidation tin plating electrolyte, comprise following component: indium, gallium, phosphorus, stannum.Wherein, with the weight of stannum
On the basis of, the percentage by weight of indium is 0.005%-0.04%, and the percentage by weight of gallium is 0.005%-0.06%, the weight of phosphorus
Percentage ratio is 0.01%-0.05%.
Embodiment 1
Take 100g tin plating electrolyte two parts, be designated as 1#, 2# respectively, under conditions of temperature 230 DEG C, add in 1# tin plating electrolyte simultaneously
Enter indium, gallium, phosphorus；Wherein, on the basis of tin plating electrolyte weight, the indium that added, gallium, the percentage by weight of phosphorus be respectively 0.01%,
0.06%, 0.02%, indium adds with the form of indium-stannum intermediate alloy, and indium content is described indium-stannum intermediate alloy quality
5%；Gallium adds with the form of gallium-stannum intermediate alloy, and 5% that gallium content is described gallium-stannum intermediate alloy quality；Phosphorus with phosphorus-
The form of stannum intermediate alloy adds, and 5% that phosphorus content is described phosphorus-stannum intermediate alloy quality.
2# tin plating electrolyte is blank group, and 1#, 2# tin plating electrolyte aoxidizes 5 hours respectively, and (oxidizing condition is: room temperature is heated to
230 DEG C, constant temperature after 5 hours air cooling to room temperature) after, test the weight of 1#, 2# tin plating electrolyte respectively, and the weightening finish before and after being aoxidized
Amount, characterizes its antioxygenic property with gain in weight, and result of the test is as shown in table 1, as shown in Table 1, add in tin plating electrolyte indium,
Gallium, phosphorus, can be obviously improved the antioxygenic property of tin liquor.
Table 1
| Tin plating electrolyte is numbered | 1# | 2# |
| Gain in weight (g) after oxidation | 0.170 | 0.350 |
| Sprawl relative area (%) | 118 | 100 |
| Yield strength (MPa) | 66 | 65 |
| Tensile strength (MPa) | 206 | 190 |
| Fusing point (DEG C) | 181 | 183 |
Above-mentioned 1# and 2# tin plating electrolyte is detected in copper wettability of the surface, with tin plating electrolyte the paving of anaerobic red copper surface
Developable surface amasss and characterizes, and method of testing is: the red copper sheet sand papering of annealing is gone removing oxide layer, and cleans with ethanol, take
10g tin plating electrolyte is placed on red copper sheet, covers with Colophonium or other scaling powders, is warming up to 230 DEG C, takes out, treat cold after insulation 60s
But measuring spreading area (use camera to take pictures, and utilize Imge-Pro plus computed in software area) to room temperature, 1# and 2# plates
The wettability test of tin liquor respectively does 3 groups, and spreading area takes its meansigma methods, with the wetting areas of 2# blank group is
The moistening relative area of 100% conversion 1# tin plating electrolyte, result of the test is shown in Table 1.As shown in Table 1, the wettability of 1# tin plating electrolyte with
The wettability of blank group tin plating electrolyte has been compared and has been promoted by a small margin, it is seen that after adding indium, gallium, phosphorus in tin liquor simultaneously, indium,
Gallium, phosphorus can work in coordination with generation effect, improve the wettability of tin plating electrolyte.
Testing the fusing point of above-mentioned 1# and 2# tin plating electrolyte test specimen, fusing point uses differential scanning calorimeter (DSC) to carry out
Test, test result is shown in Table 1.As shown in Table 1, tin liquor is added indium, gallium, phosphorus simultaneously, the fusing point of tin plating electrolyte test specimen is slightly dropped
Low.
Yield strength and tensile strength to above-mentioned 1# and 2# tin plating electrolyte test specimen are tested, and method of testing is routine side
Method, test result is shown in Table 1.As shown in Table 1, after tin liquor adds indium, gallium, phosphorus simultaneously, to the yield strength of tin plating electrolyte test specimen and
Tensile strength does not the most produce impact.
Comparative example 1
Take 100g tin plating electrolyte five parts, numbered 1#, 2#, 3#, 4#, and under conditions of temperature 230 DEG C, in 1# tin plating electrolyte
Add the indium of tin plating electrolyte weight 0.01%, in 2# tin plating electrolyte, add the gallium of tin plating electrolyte weight 0.06%, add in 3# tin plating electrolyte
Enter the phosphorus of tin plating electrolyte weight 0.02%, without any element in 4# tin plating electrolyte, as blank group, aoxidize (oxidation in 5 hours
Condition is: be heated to 230 DEG C, is incubated 5h, and air cooling is to room temperature) after test the weight of 1#, 2#, 3#, 4# tin plating electrolyte respectively, with each group
Rate of body weight gain before and after tin plating electrolyte oxidation characterizes its antioxygenic property, and result of the test is as shown in table 2.
Above-mentioned 1#, 2#, 3#, 4# tin plating electrolyte is detected in copper wettability of the surface, with tin plating electrolyte at anaerobic red copper table
The spreading area in face characterizes, and method of testing is with embodiment 1, and test result is shown in Table 2.To above-mentioned 1#, 2#, 3#, 4# tin plating electrolyte
Test specimen fusing point, yield strength and tensile strength are tested, and method of testing is with embodiment 1, and test result is shown in Table 2.
Table 2
| Tin plating electrolyte is numbered | 1# | 2# | 3# | 4# |
| Gain in weight (g) after oxidation | 0.235 | 0.221 | 0.272 | 0.244 |
| Sprawl relative area (%) | 111 | 93 | 102 | 100 |
| Yield strength (MPa) | 65 | 65 | 65 | 65 |
| Tensile strength (MPa) | 190 | 190 | 190 | 190 |
As shown in Table 2, tin plating electrolyte adds indium or gallium or phosphorus, all antioxygenic property to tin plating electrolyte have carrying by a small margin
Rise.The oxidation test result of comparative example 1 understands, the antioxygenic property of the antioxidation tin plating electrolyte based on indium gallium phosphorus of the application
It is substantially better than and is individually added into the antioxygenic property of tin plating electrolyte after indium, gallium, phosphorus.
As shown in Table 2, the wettability of tin plating electrolyte is slightly reduced by the membership that adds of gallium, the addition of the indium wettability to tin plating electrolyte
Slightly promote, and the addition of phosphorus on tin plating electrolyte wettability almost without impact.Can with the wettability test Comparative result of embodiment 1
Know, be simultaneously introduced in tin plating electrolyte indium, gallium, phosphorus kamash alloy than the wettability of kamash alloy being individually added into indium, gallium, phosphorus
Excellence, this explanation indium, gallium, three kinds of kamash alloys of phosphorus produce synergism in tin plating electrolyte, and it is with the use of the profit to tin plating electrolyte
Wet performance promotes has good effect.
Meanwhile, from Table 2, it can be seen that tin plating electrolyte adds indium, gallium, phosphorus, all fusing point and the physical force to tin plating test specimen
Learn performance no impact.But compare with embodiment 1, it is found that in tin plating electrolyte, be simultaneously introduced the tinbase conjunction of indium, gallium, phosphorus
Gold can obviously reduce the fusing point of tin plating test specimen, but does not affect yield strength and the tensile strength of tin plating test specimen, and this is for by this Shen
The application on photovoltaic welding belt of the antioxidation tin plating electrolyte based on indium gallium phosphorus please is significant.
Embodiment 2
The present embodiment, as a example by industry tin-coated copper production line, fills the stannum melt of 80kg in the stannum stove of tin-coated copper production line,
Temperature is 225-240 DEG C, when stirring starts, adds 5% indium-stannum intermediate alloy in the stannum stove filling 80kg stannum melt
0.16kg-0.64kg, 5% gallium-stannum intermediate alloy 0.16kg-0.96kg, 5% phosphorus-stannum intermediate alloy 0.32kg-0.64kg, i.e.
Obtain antioxidation tin plating electrolyte；Then with 80-120m/min speed, anaerobic copper belt is carried out hot tinning.
Comparative example 2
The present embodiment, as a example by industry tin-coated copper production line, fills the stannum melt of 80kg in the stannum stove of tin-coated copper production line,
Temperature is 225-240 DEG C, directly to anaerobic copper belt, stannum melt is carried out hot tinning with 80-120m/min speed.This production line
Within four months, the accumulative scruff that produces of all-in-one amounts to 2891kg, scruff accounting rate about 0.63%, and semiautomatic loading mechanism is accumulative produces block tin altogether
Meter 13902kg, block tin accounting rate 17.99%.
Embodiment 2 is compared with this comparative example 2, and scruff accounting rate maximum can drop to about 0.3%, and block tin accounting rate is
About 12% can be dropped to greatly, substantially increase the utilization rate of stannum and improve the lumber recovery of tinned wird, decreasing life simultaneously
" dragging for slag " operation during product, improves productivity ratio.
The sample of embodiment 2 and comparative example 2 is carried out salt spray test, and the condition of salt spray test is as follows: temperature 35 DEG C, humidity
More than 90%, concentration is the NaCl solution of 10%, and test period is 48 hours.The corrosion condition of each test specimen after observation accelerated corrosion
Understanding, the test specimen of comparative example, under salt mist environment, occurs oxidation black speck successively, and the test specimen of embodiment 2 is little 72 after 48 hours
A small amount of stain only occurred time after.
To sum up, in the present invention, adding indium, gallium, three kinds of elements of phosphorus in tin liquor, these three element can be at tin liquor Surface Creation
The oxide-film of a kind of densification, hinders oxygen atom to tin liquor diffusion inside, prevents the continuation of tin liquor from aoxidizing, thus be effectively improved tin plating
The antioxygenic property of liquid, slightly promotes the wettability of tin plating electrolyte meanwhile, decreases the fusing point of tin-plated product, and not
Affect other physical and mechanical properties of tin-plated product.
Although, in this specification, the present invention is described in detail the most with a general description of the specific embodiments,
But on the basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.
Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed model
Enclose.
Claims (8)
1. an antioxidation tin plating electrolyte based on indium gallium phosphorus, it is characterised in that comprise following component: indium, gallium, phosphorus, stannum.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 1, it is characterised in that be with the weight of described stannum
Benchmark, the percentage by weight of described indium is 0.005%-0.04%, and the percentage by weight of described gallium is 0.005%-0.06%, institute
The percentage by weight stating phosphorus is 0.01%-0.05%.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 2, it is characterised in that the weight percent of described indium
Ratio is 0.01%-0.04%.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 2, it is characterised in that the weight percent of described gallium
Ratio is 0.01%-0.06%.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 2, it is characterised in that the weight percent of described phosphorus
Ratio is 0.02%-0.04%.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 1, it is characterised in that described indium is with in indium-stannum
Between the form fusing described antioxidation tin plating electrolyte based on indium gallium phosphorus of preparation of alloy.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 1, it is characterised in that described gallium is with in gallium-stannum
Between the form fusing described antioxidation tin plating electrolyte based on indium gallium phosphorus of preparation of alloy.
Antioxidation tin plating electrolyte based on indium gallium phosphorus the most according to claim 1, it is characterised in that described phosphorus is with in phosphorus-stannum
Between the form fusing described antioxidation tin plating electrolyte based on indium gallium phosphorus of preparation of alloy.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610789854.1A CN106119755B (en) | 2016-08-31 | 2016-08-31 | A kind of anti-oxidant tin plating electrolyte based on indium gallium phosphorus |
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| CN201610789854.1A CN106119755B (en) | 2016-08-31 | 2016-08-31 | A kind of anti-oxidant tin plating electrolyte based on indium gallium phosphorus |
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| CN106119755B CN106119755B (en) | 2019-05-17 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947920A (en) * | 2006-11-23 | 2007-04-18 | 太仓市南仓金属材料有限公司 | Lead-free anti-oxidation alloy of lead-free soldering flux, prepn. method and use thereof |
| CN1995422A (en) * | 2006-01-06 | 2007-07-11 | 罗应飞 | Environment-friendly type high temperature oxidation-resistance stannum alloy |
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- 2016-08-31 CN CN201610789854.1A patent/CN106119755B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995422A (en) * | 2006-01-06 | 2007-07-11 | 罗应飞 | Environment-friendly type high temperature oxidation-resistance stannum alloy |
| CN1947920A (en) * | 2006-11-23 | 2007-04-18 | 太仓市南仓金属材料有限公司 | Lead-free anti-oxidation alloy of lead-free soldering flux, prepn. method and use thereof |
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