CN101323064A - Oxidation-resistance Sn-Cu leadless solder - Google Patents
Oxidation-resistance Sn-Cu leadless solder Download PDFInfo
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- CN101323064A CN101323064A CNA2008101165044A CN200810116504A CN101323064A CN 101323064 A CN101323064 A CN 101323064A CN A2008101165044 A CNA2008101165044 A CN A2008101165044A CN 200810116504 A CN200810116504 A CN 200810116504A CN 101323064 A CN101323064 A CN 101323064A
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Abstract
The invention relates to an antioxidant Sn-Cu lead-free solder belonging to the technical field of electronic assembly solder materials. Existing antioxidant Sn-Cu lead-free solder has high cost, weak oxidation resistance and other problems. The components and the weigh percentages of the components of the antioxidant Sn-Cu lead-free solder provided by the invention are as follows: 0.1-1.5 percent of Cu, 0.01-1 percent of Ni, 0.01-1 percent of Ce, 0.001-1 percent of P, 0.0001- 0.1 percent of Ga and the rest of Sn. The antioxidant Sn-Cu lead-free solder is obtained by adopting the Sn-Cu alloy of comparatively low cost and adding trace elements; compared with traditional Sn-Cu lead-free solder, the invention has the advantages of high anti-oxidation, little slag, relatively low cost and excellent service performance; meanwhile, the invention has wide application prospect in electronic assembly wave soldering.
Description
Technical field
The invention belongs to electronics assembling and soldering material manufacturing technology field, be specifically related to a kind of oxidation-resistance Sn-Cu leadless solder.
Background technology
Continuous implementation along with WEEE (Waste Electrical and Electronic Equipment) and RoHS (TheRestriction of the Use of certain Hazardous Substances in Electrical andElectronic Equipment) instruction, electronics assembling and soldering material unleaded started new overbearing tide, in order to seek the substitute of electronics assembling Sn-Pb solder, relevant expert has carried out a large amount of research both at home and abroad, and has obtained certain effect.At present, modal lead-free brazing mainly contains: series alloy solders such as Sn-Bi, Sn-Ag, Sn-Cu, Sn-Zn, Sn-Ag-Cu.Wherein, Sn-Cu series alloy solder has at home and abroad obtained in the Research of Lead-free Solders using widely because of characteristics with low cost.But the antioxygenic property of this series alloy solder when wave-soldering still exists certain problem.
At present, the technology of existing multiple raising lead-free brazing antioxygenic property, a kind of Sn-(5～20%) Zn-(0.2～5%) Al-(0～2.5%) Sb-(0～1.5%) Cu lead-free brazing is disclosed as ZL03116488.9, this invention is by adding the Al element, configure the accurate eutectic alloy of Sn-Zn-Al ternary with antioxygenic property, thereby correspondingly improved the antioxygenic property of brazing filler metal alloy, but at present on producing practical application still less.ZL03126796.3 discloses a kind of Sn-(0.05～1.2%) Ag-(0.5～10%) Bi-(0.01～1.5%) Cu-(0.0001～0.0009%) P-(0.002～0.8%) RE lead-free brazing, and this invention is by adding P and Sn, the O of trace
2Generate the promptly thin fine and close again oxysalt diaphragm of one deck Deng element, thereby improve the antioxygenic property on solder surface, yet, because of adding the Ag element, increase the manufacturing and the use cost of solder, and the interpolation of Bi also is easy to generate segregation.ZL03110895.4 provides a kind of Sn-(0.5～5%) Ag-(0～2%) Cu-(0.001～1%) P oxidation resistant lead-free solder, the Sn-Ag-Cu series alloy is adopted in this invention, improve the antioxygenic property of solder surface by the kelvin effect of P on the solder alloy molten surface, but the Sn-Ag-Cu series alloy is compared with the Sn-Cu series alloy, and still cost is higher.ZL03111446.6 and ZL03134099.7 disclose Sn-(0.1～2.0%) Cu-(0.001～1%) P lead-free brazing and Sn-(0.5～0.7%) Cu-(0.001～0.1%) X oxidation resistant lead-free solder (wherein X refers to Ge and/or P) respectively, the antioxygenic property of these two invention lead-free brazings can satisfy instructions for use substantially, but the brightness on lead-free solder alloy surface is not good enough, and antioxygenic property can only be within certain limit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, and a kind of antioxygenic property height, slag yield is low, cost the is low Sn-Cu eutectic lead-free brazing that is used for wave-soldering are provided.
The present invention is by adding micro-Ni, Ce, P and Ga in traditional Sn-Cu alloy, obtain oxidation-resistance Sn-Cu leadless solder, its component and shared percentage by weight thereof are: Cu 0.1～1.5%, Ni0.01～1%, Ce 0.01～1%, P 0.001～1%, Ga 0.0001～0.1%, surplus are Sn.
The selection principle of lead-free solder alloy element of the present invention is as follows:
1) Sn-Cu alloy: have relatively low cost, the raw material supply abundance, composition is simple.Sn and Cu are eutectic or nearly eutectic composition, and the brazing filler metal alloy element reclaims easily.Simultaneously, the Sn-Cu eutectic alloy has advantages such as high heat conductance, low-resistivity, mechanical property be reliable again, is a kind of extremely practical lead-free solder alloy.
2) Ni: add micro-Ni and can form Ni with Sn
3Sn, Ni
3Sn
2, Ni
3Sn
4Three kinds of intermetallic compounds, thus Cu suppressed
6Sn
5The growth of intermetallic compound.Ni can significantly shorten the wetting time of solder on copper base, improves wetting power, improves the spreading property of Sn-Cu solder effectively.The Ni that adds trace can make the spiculation compound Cu on molten solder surface
6Sn
5Englobement is significantly improved the solder flowability, suppresses the generation of crest solder joint bad phenomenon such as " bridgings ", thereby obtains good soldering effect, and the adding of Ni simultaneously also can suppress the dissolving of Cu in solder.In addition, add Ni and have the effect that reduces the scolding tin quantity of slag, Ni is gradually stably as the interpolation element of wave-soldering with lead-free brazing.
3) Ce: add the mechanical property that micro-Ce can obviously improve solder, and the wetting and spreading performance of solder is not had influence.Research has been found that an amount of Elements C e can suppress the generation of pin/sheet eutectic structure, crystal grain thinning tissue effectively.Ce and Sn easily form compound at the crystal boundary place of matrix, and these dystectic stable compounds can become small heterogeneous body nucleus in the solder cooling procedure, thereby play the effect of crystal grain thinning.Add the Ce element of trace in the Sn-Cu solder, the microscopic structure of solder obtains refinement, and its tensile property, creep-resistant property and microhardness are improved largely.
4) P: add micro-P and can make the liquid solder surface that better antioxidation is arranged in welding process.Because P has formed fine and close surface protection film on the liquid solder surface by autoxidation, has reduced the oxide that produces tin owing to the liquid tin oxidation, thereby has reduced the generation of surperficial scruff.When the addition of P element in the Sn-Cu solder alloy was less than 0.001%, antioxidation was not obvious; When the addition of P element surpassed 1%, excessive P element can have a strong impact on the soldering processes performance of solder.
5) Ga: add micro-Ga and can make the liquid solder surface that good antioxidation is arranged, but the time of keeping is shorter.The addition of Ga element is less than at 0.0001% o'clock in the Sn-Cu solder alloy, and antioxidation is not obvious; When the addition of Ga element surpasses 0.1%, will reduce the processing performance of solder, and increase the solder cost.
Oxidation-resistance Sn-Cu leadless solder provided by the present invention can be by traditional method of smelting preparation, wherein Sn, Cu, Ni, Ce are with the raw metal supply, and P (44 ℃) and Ga (29.8 ℃) are lower because of fusing point, in the easy extremely scaling loss of high temperature, be difficult to guarantee the addition of trace element in alloy during the preparation brazing filler metal alloy, therefore, P and Ga add with the form of intermediate alloy PCu and SnGa.
Compare with existing anti-oxidant Sn-Cu lead-free brazing, solder of the present invention has following beneficial effect:
1) the present invention adopts to add micro-P and Ga simultaneously in the Sn-Cu solder alloy, when the antioxidation of assurance Ga element is given full play to, adopts element P to increase the action time of the antioxygen of Ga element.
2) the prepared solder of the present invention has excellent antioxygenic property when the high temperature wave-soldering, and the liquid solder pond can keep antioxidant status for more time, and soldering solder joint surface-brightening is attractive in appearance.
3) the present invention has reduced the quantity of the oxidizing slag that produces in the solder use, thereby has reduced the consumption of Sn, reduces production costs.
4) lead-free brazing of the present invention can adopt traditional processing technology to make soldering tin bar, scolding tin rod, solder stick, solder ball and soldering paste etc., has broad application prospects in electronics assembling wave-soldering.
The invention will be further described below in conjunction with the specific embodiment.
The specific embodiment
Embodiment 1
1) salt-mixtures with 26 gram potassium chloride and 20 grams lithium chlorides water on 99.874 gram tin after the fusing down at 450 ℃, and furnace temperature is risen to 600 ℃, treat the tin fusing after, add 0.094 gram copper, constantly stir, form molten alloy;
2) 0.01 gram nickel, 0.01 gram cerium, 0.007 gram PCu intermediate alloy and 0.005 gram SnGa intermediate alloy are pressed into rapidly in the molten alloy in the step 1) with glass bar, and constantly stir, until fusing fully, be incubated 2 hours, constantly stir, make the alloy homogenising, leave standstill and come out of the stove, treat to remove surperficial salt-mixture behind the alloy graining, obtain the solder piece;
3) furnace temperature is reduced to 350 ℃ the solder piece reheated fusing after, the solder liquid of molten state is watered in the strip mould, cooling obtains oxidation-resistance Sn-Cu leadless solder fast, component and content thereof see Table in 1.
Embodiment 2
1) salt-mixtures with 26 gram potassium chloride and 20 grams lithium chlorides water on 91.0 gram tin after the fusing down at 450 ℃, and furnace temperature is risen to 600 ℃, treat the tin fusing after, add 0.94 gram copper, constantly stir, form molten alloy;
2) 1 gram nickel, 1 gram cerium, 0.7 gram PCu intermediate alloy and 5 gram SnGa intermediate alloys are pressed into rapidly in the molten alloy in the step 1) with glass bar, and constantly stir, until fusing fully, be incubated 2 hours, constantly stir, make the alloy homogenising, leave standstill and come out of the stove, treat to remove surperficial salt-mixture behind the alloy graining, obtain the solder piece;
3) furnace temperature is reduced to 350 ℃ the solder piece reheated fusing after, the solder liquid of molten state is watered in the strip mould, cooling obtains oxidation-resistance Sn-Cu leadless solder fast, component and content thereof see Table in 1.
Embodiment 3
1) salt-mixtures with 26 gram potassium chloride and 20 grams lithium chlorides water on 93.998 gram tin after the fusing down at 450 ℃, and furnace temperature is risen to 600 ℃, treat the tin fusing after, add 0.78 gram copper, constantly stir, form molten alloy, obtain the solder piece;
2) 0.1 gram nickel, 0.1 gram cerium, 0.022 gram PCu intermediate alloy and 5 gram SnGa intermediate alloys are pressed into rapidly in the molten alloy in the step 1) with glass bar, and constantly stir, until fusing fully, be incubated 2 hours, constantly stir, make the alloy homogenising, leave standstill and come out of the stove, treat to remove surperficial salt-mixture behind the alloy graining;
3) furnace temperature is reduced to 350 ℃ the solder piece reheated fusing after, the solder liquid of molten state is watered in the strip mould, cooling obtains oxidation-resistance Sn-Cu leadless solder fast, component and content thereof see Table in 1.
Embodiment 4
1) salt-mixtures with 26 gram potassium chloride and 20 grams lithium chlorides water on 98.42 gram tin after the fusing down at 450 ℃, and furnace temperature is risen to 600 ℃, treat the tin fusing after, add 0.6 gram copper, constantly stir, form molten alloy;
2) 0.08 gram nickel, 0.15 gram cerium, 0.7 gram PCu intermediate alloy and 0.05 gram SnGa intermediate alloy are pressed into rapidly in the molten alloy in the step 1) with glass bar, and constantly stir, until fusing fully, be incubated 2 hours, constantly stir, make the alloy homogenising, leave standstill and come out of the stove, treat to remove surperficial salt-mixture behind the alloy graining, obtain the solder piece;
3) furnace temperature is reduced to 350 ℃ the solder piece reheated fusing after, the solder liquid of molten state is watered in the strip mould, cooling obtains oxidation-resistance Sn-Cu leadless solder fast, component and content thereof see Table in 1.
Embodiment 5
1) salt-mixtures with 26 gram potassium chloride and 20 grams lithium chlorides water on 99.06 gram tin after the fusing down at 450 ℃, and furnace temperature is risen to 600 ℃, treat the tin fusing after, add 0.14 gram copper, constantly stir, form molten alloy;
2) 0.15 gram nickel, 0.08 gram cerium, 0.07 gram PCu intermediate alloy and 0.5 gram SnGa intermediate alloy are pressed into rapidly in the molten alloy in the step 1) with glass bar, and constantly stir, until fusing fully, be incubated 2 hours, constantly stir, make the alloy homogenising, leave standstill and come out of the stove, treat to remove surperficial salt-mixture behind the alloy graining, obtain the solder piece;
3) furnace temperature is reduced to 350 ℃ the solder piece reheated fusing after, the solder liquid of molten state is watered in the strip mould, cooling obtains oxidation-resistance Sn-Cu leadless solder fast, component and content thereof see Table in 1.
Comparative Examples
For comparing the prepared oxidation-resistance Sn-Cu leadless solder of the present invention and the antioxygenic property of existing lead-free brazing, adopting the Sn-Cu lead-free brazing that adds trace element as shown in table 2 is Comparative Examples.
Respectively the solder for preparing among embodiment 1-5 and the Comparative Examples 1-14 is placed crucible, under atmospheric conditions, be heated to experimental temperature after, observe the variation of its surface color, antioxidant effect and slag yield are as shown in table 3, slag yield calculates according to formula (1).
Formula (1)
| Composition | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Cu | 0.1 | 1.5 | 0.8 | 1.2 | 0.2 |
| Ni | 0.01 | 1 | 0.1 | 0.08 | 0.15 |
| Ce | 0.01 | 1 | 0.1 | 0.15 | 0.08 |
| P | 0.001 | 0.1 | 0.003 | 0.1 | 0.01 |
| Ga | 0.0001 | 0.1 | 0.1 | 0.001 | 0.01 |
| Sn | Surplus | Surplus | Surplus | Surplus | Surplus |
The component of prepared oxidation-resistance Sn-Cu leadless solder and content % among table 1, the embodiment 1-5
| Composition | P | Ge | RE | Ga |
| Comparative Examples 1 | 0.001 | |||
| Comparative Examples 2 | 0.01 | |||
| Comparative Examples 3 | 0.1 | |||
| Comparative Examples 4 | 0.001 | |||
| Comparative Examples 5 | 0.01 | |||
| Comparative Examples 6 | 0.1 | |||
| Comparative Examples 7 | 0.05 | |||
| Comparative Examples 8 | 0.1 | |||
| Comparative Examples 9 | 0.5 | |||
| Comparative Examples 10 | 0.0001 | |||
| Comparative Examples 11 | 0.001 | |||
| Comparative Examples 12 | 0.01 | |||
| Comparative Examples 13 | 0.01 | 0.01 | ||
| Comparative Examples 14 | 0.01 | 0.1 |
The trace element and the addition % thereof that are added in the Sn-Cu lead-free brazing among table 2, the Comparative Examples 1-14
| The trace element composition | Heating-up temperature (℃) | Retention time (h) | The situation of solder oxidation rear surface | Slag yield (%) | |
| Comparative Examples | P | 280 | 24 | Brightness is higher | 1.596 |
| Comparative Examples 2 | P | 280 | 24 | Brightness is higher, presents metallic luster | 1.542 |
| Comparative Examples 3 | P | 280 | 24 | Brightness is higher | 1.553 |
| Comparative Examples 4 | Ge | 280 | 24 | Brightness is higher, surperficial little rough | 0.823 |
| Comparative Examples 5 | Ge | 280 | 24 | Brightness is higher, and metallic luster is silvery white in color | 0.808 |
| Comparative Examples 6 | Ge | 280 | 24 | Brightness is higher, oxidation skin depth, smooth surface | 0.815 |
| Comparative Examples 7 | RE | 280 | 24 | Almost do not have brightness, the surface is bronzing | 4.699 |
| Comparative Examples 8 | RE | 280 | 24 | Almost there is not brightness | 4.687 |
| Comparative Examples 9 | RE | 280 | 24 | Almost do not have brightness, the surface is pitch-black | 4.932 |
| Comparative Examples 10 | Ga | 280 | 24 | Almost do not have brightness, rough surface is black | 1.999 |
| Comparative Examples 11 | Ga | 280 | 24 | Almost do not have brightness, the surface is black | 1.930 |
| Comparative Examples 12 | Ga | 280 | 24 | Almost do not have brightness, the surface is black | 1.908 |
| Comparative Examples 13 | P+Ge | 280 | 24 | Brightness is higher | 1.040 |
| Comparative Examples 14 | P+RE | 280 | 24 | Brightness is general | 4.624 |
| Embodiment 1 | P+Ga+Ni+Ce | 280 | 24 | Brightness is high, and oxide skin as thin as a wafer | 0.7567 |
| Embodiment 2 | P+Ga+N i+Ce | 280 | 24 | Brightness is high, presents metallic luster | 0.7432 |
| Embodiment 3 | P+Ga+Ni+Ce | 280 | 24 | Brightness is high, and oxide skin is thinner | 0.7703 |
| Embodiment 4 | P+Ga+Ni+Ce | 280 | 24 | Brightness is high, smooth surface | 0.7551 |
| Embodiment | P+Ga+Ni+Ce | 280 | 24 | Brightness is the highest, and the surface presents metallic luster | 0.7329 |
(* experiment solder is 100g, and the oxidized surface that solder contacts with atmosphere is long-pending to be 2640mm for the antioxygenic property of prepared solder and slag yield among table 3, Comparative Examples 1-14 and the embodiment 1-5
2)
Claims (1)
1, a kind of oxidation-resistance Sn-Cu leadless solder, it is characterized in that the component of described solder and shared percentage by weight thereof are: Cu 0.1～1.5%, Ni 0.01～1%, Ce 0.01～1%, P 0.001～1%, Ga 0.0001～0.1%, surplus are Sn.
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| CNA2008101165044A CN101323064A (en) | 2008-07-11 | 2008-07-11 | Oxidation-resistance Sn-Cu leadless solder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664861B (en) * | 2009-09-21 | 2012-02-01 | 天津大学 | Sn-Cu based lead-free solder alloy with improved solder joint creep property and preparation technology thereof |
| CN103084750A (en) * | 2013-02-25 | 2013-05-08 | 重庆科技学院 | High-melting-point lead free brazing filler metal used for electronic packaging and preparation method thereof |
| CN105252163A (en) * | 2015-11-13 | 2016-01-20 | 广东中实金属有限公司 | Lead-free tin-soldering wire applied to automatic soldering robot and preparation method thereof |
| CN110303269A (en) * | 2019-07-02 | 2019-10-08 | 华侨大学 | For the Sn-Cu-Ti solder of low temperature brazing diamond and application |
| CN115156755A (en) * | 2022-08-12 | 2022-10-11 | 云南锡业集团（控股）有限责任公司研发中心 | Sn-Ag-Cu lead-free solder containing Bi, ni and Ga and preparation method thereof |
-
2008
- 2008-07-11 CN CNA2008101165044A patent/CN101323064A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664861B (en) * | 2009-09-21 | 2012-02-01 | 天津大学 | Sn-Cu based lead-free solder alloy with improved solder joint creep property and preparation technology thereof |
| CN103084750A (en) * | 2013-02-25 | 2013-05-08 | 重庆科技学院 | High-melting-point lead free brazing filler metal used for electronic packaging and preparation method thereof |
| CN103084750B (en) * | 2013-02-25 | 2016-07-06 | 重庆科技学院 | A kind of preparation method of high-melting point lead-free solder used for electronic packaging |
| CN105252163A (en) * | 2015-11-13 | 2016-01-20 | 广东中实金属有限公司 | Lead-free tin-soldering wire applied to automatic soldering robot and preparation method thereof |
| CN110303269A (en) * | 2019-07-02 | 2019-10-08 | 华侨大学 | For the Sn-Cu-Ti solder of low temperature brazing diamond and application |
| CN115156755A (en) * | 2022-08-12 | 2022-10-11 | 云南锡业集团（控股）有限责任公司研发中心 | Sn-Ag-Cu lead-free solder containing Bi, ni and Ga and preparation method thereof |
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