CN102337422B - A kind of high temperature bends down the unleaded application warding off tin alloy of corrode - Google Patents
A kind of high temperature bends down the unleaded application warding off tin alloy of corrode Download PDFInfo
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- CN102337422B CN102337422B CN201010232451.XA CN201010232451A CN102337422B CN 102337422 B CN102337422 B CN 102337422B CN 201010232451 A CN201010232451 A CN 201010232451A CN 102337422 B CN102337422 B CN 102337422B
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- tin
- alloy
- unleaded
- warding
- copper
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- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 21
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052802 copper Inorganic materials 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims abstract 2
- 239000003963 antioxidant agent Substances 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 235000006708 antioxidants Nutrition 0.000 claims 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 46
- 239000010949 copper Substances 0.000 abstract description 44
- 229910020938 Sn-Ni Inorganic materials 0.000 abstract description 11
- 229910008937 Sn—Ni Inorganic materials 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 238000004090 dissolution Methods 0.000 description 10
- 229910000765 intermetallic Inorganic materials 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000009713 electroplating Methods 0.000 description 5
- 230000005496 eutectics Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 229910020888 Sn-Cu Inorganic materials 0.000 description 2
- 229910019204 Sn—Cu Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001174 tin-lead alloy Inorganic materials 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005441 electronic device fabrication Methods 0.000 description 1
- 239000006023 eutectic alloy Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical compound [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Coating With Molten Metal (AREA)
Abstract
The invention belongs to electronics and electrical device manufacturing field, relate to the tin-based alloy that electronics and electric elements leg surface high-temp hot tinning (warding off tin) use, specifically a kind of Sn-Ni base high temperature bends down the unleaded application warding off tin alloy of corrode.The chemical constitution of alloy is NiO.1-1.5%, and third element content is that (third element refers to Ag to 0.001-0.1, Cu, Si, P, Ge, Al, one or more compounds in Ga, Ti), all the other are Sn and inevitable impurity (above all by weight percentage).Compared with common tin alloy, advantage of the present invention is that this wards off tin alloy not containing heavy metal lead, simultaneously higher ward off Xi Wendu under (300-400 DEG C), slow to the corrosion speed of Copper substrate, under can being widely used in hot conditions, the unleaded of various piece surface wards off process of tin, comprises Cu, Fe, Al and their alloy, the high-temp leadless being specially adapted to undersized Cu or Cu alloy surface wards off process of tin.
Description
Technical field
The invention belongs to electronics and electrical device manufacturing field, relate to the tin-based alloy that electronics and electric elements leg surface high-temp hot tinning (warding off tin) use, specifically a kind of Sn-Ni base high temperature bends down the unleaded application warding off tin alloy of corrode.
Background technology
In electronics and electrical equipment process industry field, carrying out soldering with tin-based solder is one of the most frequently used interconnection technique, is mainly used in the electrical and mechanical connection between metal and metal.In modern industry, copper is conducting metal best at present, and therefore soldering is mainly used to the connection of Copper and its alloy.Owing to placing under field conditions (factors), there is the natural oxide film of one deck in copper or copper alloy surface, and when actual welding, the tin solder of melting is not easily having the Copper base material surface spreading of oxide film with wetting.In order to overcome this shortcoming, modern industry generally adds one leg electroplating surfaces with tin technique in electronic device fabrication processes to be solved, copper or copper alloy surface zinc-plated after, the tinsolder of melting greatly improves in the wettability of tinned surface, ensure that follow-up mother metal has good weldability thus.
At present, the electroplating surfaces with tin technique of copper or copper alloy mainly contains plating or hot dip process two kinds, and the latter wards off tin industrial also title.Generally speaking, electroplating technology is relatively complicated, and it not only requires that part to be plated has good surface to prepare, the plating conditions accurately controlled, but also will have certain plating posttreatment; In addition, the discharge of electroplating effluent also relates to the cost for wastewater treatment of great number, and particularly each major industrial country of the world improves emission standard in succession at present, and therefore the production cost of eleetrotinplate has the trend significantly risen.As a comparison, ward off process of tin relatively simple, it is the tin or the tin alloy that Copper substrate (copper wire, copper sheet etc.) are directly immersed high-temperature fusion, reacted by solid/liquid interfaces, be stained with after one deck tin until surface, take out from the tin of high-temperature fusion rapidly, solidify rear formation surface heat tin coating.This technique does not generally need follow-up surface treatment, does not have the problem that electroplating wastewater discharges yet, and is therefore a kind of energy-saving and emission-reducing technique.Along with the attention gradually of Environmental pollution problem, can predict, in the future in this area, high temperature is warded off process of tin and will be had very strong technological competitiveness.
Traditional heat wards off tin alloy mainly eutectic tin-lead alloy (Sn63%-Pb37%), and its fusing point is 183 DEG C, and the good fluidity of the lower and eutectic alloy of the raw materials cost due to this alloy itself, is thus once widely used by industry member.In recent years, because countries in the world government to cause the attention of problem of environmental pollution to using heavy metal lead in electronics and electrical equipment industry, countries in the world are in succession to the restriction that used heavy metal lead to carry out in electronics and electrical equipment industry or forbid.Through a large amount of scientific researches, current industry member has been developed some lead-free alloys and has been substituted original eutectic tin-lead alloy.Such as, tin is warded off on Cu matrix, main with Sn-Cu alloy for representative, lead-free alloy conventional is at present eutectic or hypereutectic gun-metal, copper content is 0.7wt%-4wt%, wherein the Main Function of alloy element copper is the dissolution rate reduced when high temperature wards off tin in the liquid tin of Copper substrate, the principles of science of its foundation be a kind of solid metal in the melt close to self saturation solubility, not easily dissolved again due to the dissolution equilibrium of solid/liquid interfaces.
The subject matter adopting eutectic or hypereutectic tin copper lead-free alloy to carry out running into when heat wards off tin operation is the restriction to warding off Xi Wendu, according to copper-Xi binary phase diagram, Sn-Cu eutectic point is 227 DEG C (containing Cu0.7wt%), when the temperature increases, the saturation solubility of copper in tin will sharply raise, when warding off Xi Wendu and reaching 300 DEG C, the saturation solubility of copper in tin is close to 4%, and temperature is when reaching 400 DEG C, the saturation solubility of copper in liquid tin will close to 8%, because a large amount of copper dissolutions is in liquid tin, increase the melt viscosity of hypereutectic alloy, the latter sharply reduces again the liquid fluidity of alloy itself, very large difficulty is caused thus to warding off tin operation, therefore copper content is unsuitable too high.And the Sn-4%Cu alloy higher for copper content, ward off Xi Wendu no more than 300 DEG C, otherwise the dissolution rate of Copper substrate in liquid tin sharply will rise.
But, often need to carry out warding off tin operation under the high temperature more than 300 DEG C in electronics and electrical equipment industry, particularly tin is warded off with the thin copper wire surface of enameled wire in some surfaces, require in production that thin copper wire directly carries out surface and wards off tin when not removing surperficial paint film, to reduce relevant process procedure, save production cost.Production practice show, the paint film general requirement of enamelled wire surface immerses in the hot tin of 350-400 DEG C of high temperature could be removed rapidly, therefore relevant industrial requires that the Xi Wendu that wards off of alloy brings up to this temperature range, so that the technical requirements that tin is warded off on surface is directly carried out in satisfied production, improves production high-level efficiency.But just as previously mentioned, when warding off Xi Wendu and raising, because the saturation solubility of copper in tin also will sharply raise, at 350-400 DEG C of high temperature range, Sn-4%Cu alloy is far below its saturation solubility, and at this moment the dissolution rate of copper will increase sharply.With this understanding, the copper wire thinner for some diameters, ward off in tin process, the control of immersing the time must be very strict, and the time is too short, surface paint film not yet removes, the not yet sticky tin in copper wire surface, and the time is slightly long, because the high speed of copper is dissolved, copper wire dissolves completely in molten tin, and both all cause and ward off tin failure.Therefore, how effectively reducing the solubleness of copper in molten tin alloy under high temperature is that current high temperature wards off one of key problem in technology that urgently will solve in process of tin.
Summary of the invention
Warding off copper rapidly-soluble problem in liquid tin in tin process to overcome high temperature, the invention provides the low corrode leadless tin-base alloy that a kind of Gong high temperature newly wards off tin.
Main technical schemes of the present invention is:
A kind of high temperature bends down the unleaded of corrode and wards off tin alloy, by adding a small amount of nickel in industrial pure tin, form Sn-Ni base alloy, owing to containing a small amount of nickel in alloy, copper dissolution rate in tin under its effective minimizing high temperature, thus be easy to realize industrial technical need of high-temperature hot being warded off to tin.
Described high temperature bends down the unleaded of corrode and wards off tin alloy, and with Sn-Ni alloy for essentially consist, adding a small amount of third element is antioxidant addn, and the weight percent of its alloy consists of:
Ni0.1-1.5% (preferable range 0.3-1%);
Third element 0.001-0.1% (preferable range 0.005-0.05%);
Sn and inevitably impurities balance.
In the present invention, described third element refers to Ag, one or more the combination in Cu, Si, P, Ge, Ga, Al, Ti, and when several third element combines, its total amount is no more than the concentration range that its composition specifies.
High temperature provided by the invention is warded off tin alloy and a kind of common smelting technique can be selected to smelt, and can cool by ingot casting, obtain alloy product after alloy fully melts and stirs.
Know-why of the present invention is as follows:
The present invention is by finding the dissolution kinetics research of copper in high-temperature fusion tin, the dissolving of copper in liquid tin can be divided into two primary processes, when copper immerses in high-temperature liquid state tin, first form one deck copper-Sn intermetallic compound at interface and (lower than in 415 DEG C of situations, first form Cu
6sn
5, and form Cu higher than on solid-liquid interface when 415 DEG C
3sn).Then, this layer of intermetallic compound is dissolved in liquid tin more further.Two processes hocket until copper all dissolves.According to the understanding to this dissolution kinetics process, the present invention adds a small amount of nickel in liquid tin, and when copper immerses fused solution tin alloy, first the nickel dissolved in liquid state segregate to liquid/liquid/solid interface, and form one deck nickel-Sn intermetallic compound (Ni
3sn
4), this layer of new intermetallic compound has isolated copper-Sn intermetallic compound, make it can not with the contact of liquid tin, and actual what contact with liquid tin is nickel Sn intermetallic compound.Because nickel Sn intermetallic compound is more stable than copper Sn intermetallic compound, and not easily dissolved by liquid tin.Therefore, copper or the dissolution rate of copper alloy in this Sn-Ni alloy are just effectively suppressed.According to this principle; when the addition of nickel is not enough; its can not segregation in solid/liquid interfaces; form continuous print protective layer, thus the rapid solution of copper in liquid tin under effectively can not suppressing high temperature, and when the addition of nickel is too much; solid-state nickel tin compound particle can be formed in liquid tin; affect viscosity and the mobility of liquid alloy, as previously mentioned, the liquid alloy mobility of difference will have a strong impact on the processing performance of warding off tin.
Technological merit of the present invention is:
1, the present invention is not containing heavy metal lead, is a kind of lead-free alloy of environment-friendly type;
2, alloy of the present invention can higher ward off Xi Wendu (350-400 DEG C) under use, in this temperature range, enameled wire top layer paint film is easy to oxidized removal; Because alloying element effectively inhibits copper dissolution rate in high-temperature liquid state tin, therefore industrial realization directly carries out without surface paint removal the object that high temperature wards off tin at the copper wire of band enameled wire, and the latter likely will significantly reduce the production cost warding off process of tin.
3, compared with common tin alloy, the present invention is slow to the corrosion speed of Copper substrate, and under can being widely used in hot conditions, the unleaded of various piece surface wards off process of tin, comprise Cu, Fe, Al and their alloy, the high-temp leadless being specially adapted to undersized Cu or Cu alloy surface wards off process of tin.
Embodiment
Embodiment 1:
By weight percentage, preparation Ni0.5%, Ag0.01%, Ga0.01%, Si0.005%, all the other are the Sn-Ni alloy of Sn, a kind of common smelting technique is selected to be melted by technical pure Sn, then add the various alloying elements weighed up by weight percentage, be fully dissolved in after in LIQUID Sn until it, stirring also, ingot casting is for subsequent use.
Get this alloy and be placed in an open pot, use retort furnace heat fused, and be warming up to 400 DEG C of insulations 30 minutes, make LIQUID Sn alloy temperature homogenizing.Get the thin copper wire (Φ 0.6mm) of a length of tape enameled wire, one end is immersed in preprepared brazing flux, take out the brazing flux that removing is unnecessary, then immerse in off-the-shelf LIQUID Sn base alloy, after 2 minutes, last layer Sn has been warded off on copper wire surface, and it is soaked 5 minutes in LIQUID Sn, and taking out the diameter measuring copper wire is 0.5mm, visible copper wire is relatively low in this Sn base alloy dissolves speed, directly wards off tin and achieves good effect.
Embodiment 2:
By weight percentage, preparation Ni1.0%, Cu0.03%, Ge0.02%, all the other are the Sn-Ni alloy of Sn, adopt the experimental technique identical with embodiment 1, directly ward off tin, achieve good effect at 400 DEG C.
Embodiment 3:
By weight percentage, preparation Ni0.3%, P0.02%, all the other are the Sn-Ni alloy of Sn, adopt the experimental technique identical with embodiment 1, directly ward off tin, achieve good effect at 350 DEG C.
Embodiment 4:
By weight percentage, preparation Ni0.5%, Al0.005%, all the other are the Sn-Ni alloy of Sn, adopt the experimental technique identical with embodiment 1, directly ward off tin, achieve good effect at 360 DEG C.
Embodiment 5:
By weight percentage, preparation Ni0.4%, Ag0.03%, Ti0.003%, all the other are the Sn-Ni alloy of Sn, adopt the experimental technique identical with embodiment 1, directly ward off tin, achieve good effect at 370 DEG C.
Embodiment 6:
By weight percentage, preparation Ni0.6%, Si0.005%, P0.01%, all the other are the Sn-Ni alloy of Sn, adopt the experimental technique identical with embodiment 1, directly ward off tin, achieve good effect at 380 DEG C.
Claims (4)
1. a high temperature bends down the unleaded application warding off tin alloy of corrode, it is characterized in that: described unleaded tin alloy of warding off is the Ni adding 0.6-1.5wt% in industrial pure tin, and anti-oxidant micro-third element, the content of anti-oxidant micro-third element is 0.001-0.1wt%;
This is unleaded ward off tin alloy be applied to hot conditions under the unleaded of various piece surface ward off process of tin, comprise Cu, Fe, Al and their alloy; Refer under described hot conditions that use temperature is 350-400 DEG C.
2. by the unleaded application warding off tin alloy described in claim 1, it is characterized in that: anti-oxidant micro-third element refers to Ag, one or more compounds in Cu, Si, P, Ge, Al, Ga, Ti.
3. by the unleaded application warding off tin alloy according to claim 1, it is characterized in that: Ni content preferable range is 0.6-1wt%.
4. by the unleaded application warding off tin alloy according to claim 1, it is characterized in that: the preferable range of anti-oxidant micro-third element content is 0.005-0.05wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010232451.XA CN102337422B (en) | 2010-07-21 | 2010-07-21 | A kind of high temperature bends down the unleaded application warding off tin alloy of corrode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010232451.XA CN102337422B (en) | 2010-07-21 | 2010-07-21 | A kind of high temperature bends down the unleaded application warding off tin alloy of corrode |
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| Publication Number | Publication Date |
|---|---|
| CN102337422A CN102337422A (en) | 2012-02-01 |
| CN102337422B true CN102337422B (en) | 2015-12-09 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105390176A (en) * | 2015-12-15 | 2016-03-09 | 北京有色金属与稀土应用研究所 | Tin-lead plating flat copper wire and preparation method thereof |
| CN107475563B (en) * | 2017-10-24 | 2019-04-12 | 河南科技大学 | One Albatra metal hot dip rare earth tin-based alloy and preparation method thereof |
| CN112736366B (en) * | 2020-12-29 | 2023-06-27 | 上海应用技术大学 | Method for cast-welding light metal negative grid lead storage battery busbar |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482266A (en) * | 2003-07-02 | 2004-03-17 | 中国科学院金属研究所 | Industrial pure tin with resistance to liquid surface oxidizing and application |
| CN1803379A (en) * | 2006-01-24 | 2006-07-19 | 昆山成利焊锡制造有限公司 | Leadless soft soldering material |
| CN101223002A (en) * | 2005-07-19 | 2008-07-16 | 斯比瑞尔社股份有限公司 | Solder free from lead for additional supply and method of regulating Cu concentration and Ni concentration in solder bath |
-
2010
- 2010-07-21 CN CN201010232451.XA patent/CN102337422B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482266A (en) * | 2003-07-02 | 2004-03-17 | 中国科学院金属研究所 | Industrial pure tin with resistance to liquid surface oxidizing and application |
| CN101223002A (en) * | 2005-07-19 | 2008-07-16 | 斯比瑞尔社股份有限公司 | Solder free from lead for additional supply and method of regulating Cu concentration and Ni concentration in solder bath |
| CN1803379A (en) * | 2006-01-24 | 2006-07-19 | 昆山成利焊锡制造有限公司 | Leadless soft soldering material |
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