CN101239425A - Leadless high-temperature electronic solder and preparation - Google Patents
Leadless high-temperature electronic solder and preparation Download PDFInfo
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- CN101239425A CN101239425A CNA2008100611669A CN200810061166A CN101239425A CN 101239425 A CN101239425 A CN 101239425A CN A2008100611669 A CNA2008100611669 A CN A2008100611669A CN 200810061166 A CN200810061166 A CN 200810061166A CN 101239425 A CN101239425 A CN 101239425A
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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
- C22C13/02—Alloys based on tin with antimony or bismuth as the next major constituent
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Abstract
A leadless hyperthermia electronic solder and preparing method thereof are disclosed. The solder is composed of alloy elements according to flowing percentage by weight: 10-224546014f Sb, 1-84550160f Cu, 0.01-224446740f Ni, 0-0.012f X, residue percent of Sn; wherein X represents zero species, one species or composition of optimal several species of Ga, P and mixed rare earth; the fusion point of the solder is between 240 DEG C to 320 DEG C, the tensile strength is 58-84MPa; the preparing method of the solder is: thermal insulating the prepared each alloy element at a temperature ranging from 850 DEG C to 900 DEG C for 1-2 hours by using a vacuum melting furnace or an antivacuum smelting furnace to melt them sufficiently, and mixing them sufficiently before discharged from the furnace, pouring, solidifying to obtain the solder; the solder is made into at least one of solder master alloy, solder block, soldered ball, soldering ring, soldering foil, soldering powder or soldering cream; the solder is provided with a higher fusion point to improve the fusion activity of solder, enhanced credibility of device, good antioxidant ability and excellent humectation performance.
Description
Technical field
That the present invention relates to is a kind of high-temperature leadless soft solder and preparation method, and especially a kind of Sn-Sb-Cu-Ni-X multi-component leadless high-temperature electronic solder and preparation method belong to welding technology field.
Background technology
In recent years, along with the raising of people's environmental consciousness with to the growing interest of self health, under the RoHS of European Union's issue instruction guiding, various countries make laws in succession and limit the use of Pb in microelectronic industry.One of so unleaded focus that becomes all circles' concern of solder, the lead-free product that replaces eutectic 63Sn-37Pb solder has been tending towards ripe and has carried out industrialization.Yet, be widely used in the high Pb solder in the high temperature field in the Electronic Packaging (Pb content greater than 85% Pb-Sn alloy) because its high melt point (about 300 ℃) and excellent comprehensive performances, also do not find at present suitable unleaded substitute, thereby in the RoHS instruction, obtained exemption.However, along with development of technology, finally realizing unleaded comprehensively in Electronic Packaging is inexorable trend, so the unleaded research of high Pb solder has important practical sense.And at present considerably less to the unleaded research of high Pb solder, that is reported in document and the patent mainly contains 80Au-Sn, Bi base alloy, Zn-A1 base alloy and Sn-Sb base alloy, but these alloys all have obvious defects separately.
The fusing point of 80Au-Sn eutectic solder is 280 ℃, and is the most close with the fusing point of high Pb solder, but this solder cost is too high, is mainly used in photoelectron encapsulation, high reliability (as the InP laser diode), high-power electronic device circuit level Hermetic Package and the chip encapsulation.
It is that the Bi-Ag alloy of 2%～18wt.% substitutes high Pb solder that Chinese patent CN155896A proposes with containing Ag, this alloy melting point is suitable, solidus temperature is greater than 262.5 ℃, but this alloy exists that fragility is big, poor in processability,, solid-liquid phase line interval broad weak with substrate combinating strength and a series of problems such as wetability difference on Cu and Ni matrix.
Although Zn-Al base alloy fusing point guarantees that than high energy solder joint does not melt in the subsequent technique, its processing characteristics and stress relaxation ability, oxidation and wetability are not good easily, and these character have limited the application of this alloy to a great extent.
Chinese patent CN1221216A proposes the Sn-Sb bianry alloy that a kind of usefulness contains Sb5～15% and is used for applying lead frame, to guarantee to bear the sealing technology of higher temperature subsequently.But the fusing point of Sn-Sb bianry alloy is relatively low when Sb content lower (＜10%), and the reliability of bearing high temperature packaging technology solder joint for needs is unfavorable.And the interfacial reaction of this alloy and Cu matrix is very fast, thereby causes the corrode especially severe of Cu.This will cause the problem of two aspects: one, Cu pad or pin are less usually in the Electronic Packaging, (3～5s) just can be all molten intact at short notice, thereby cause the inefficacy of solder joint, they are two years old, because the dissolving of Cu pad or pin also can cause the variation of liquid alloy composition, also there is bigger influence in the unstability of this composition to reliability of products.
United States Patent (USP) 20040241039 (75%Sn at least, 0.5～7%Cu, 0.05～18%Sb) and Chinese patent CN1954958A (all the other be Sn for Sb8～20%, Cu3～7%) usefulness SnSbCu ternary alloy three-partalloy has been proposed as high-temperature leadless soft solder respectively.But still there is the fast problem of corrode to Cu or Ni matrix pad in this alloy; And the antioxygenic property of this series alloy is relatively poor, can produce a large amount of scruffs in the high-temperature soldering process.
Summary of the invention
The objective of the invention is for complying with international unleaded trend, provide a kind of fusing point more than 250 ℃, and in welding process, can effectively stop Cu in the welding process or Ni pad in solder corrode and have leadless high-temperature electronic solder and preparation method than the strong anti-oxidation ability; This solder is the unleaded substitute products of high Pb solder traditional in the encapsulation field.
To achieve these goals, the invention provides a kind of Sn-Sb-Cu-Ni-X (zero kind, a kind of or several combination arbitrarily among X=Ga, P and the mishmetal) multi-component leadless solder---leadless high-temperature electronic solder.This technical scheme is to add Cu, Ni and other trace elements on the basis of Sn-Sb alloy, forms multicomponent alloy, and its weight alloy percentage consists of:
Sb： 10～22％
Cu 1～8％
Ni 0.01～2％
X 0.001％～1％
The Sn surplus
Wherein: X refers to zero kind, a kind of or several combination arbitrarily between Ga, P or the mishmetal.
Described solder fusing point between 240 ℃～320 ℃, tensile strength 58-84Mpa
A kind of preparation method of lead-free brazing as mentioned above, it is that the various alloying elements that will prepare are incubated 1～2h with vacuum melting furnace or non-vacuum melting stove down at 850～900 ℃, makes it even fusing, and fully stirs before coming out of the stove, and obtains solder behind the casting solidification.
Described solder is formed at least a in solder foundry alloy or solder piece or welding wire or soldered ball or weld-ring or weldering paper tinsel or welding powder or the soldering paste.
Know-why of the present invention is to add higher Sb content in solder, improves the fusion temperature of solder; Because the interfacial reaction speed of Sn and Cu or Ni is rapid especially under the high temperature, thereby cause the quick dissolving of Cu or Ni matrix, the adding of The addition of C u can make the melting region of solder remain on a narrower and small scope, and has reduced the dissolving of Cu or Ni matrix; The adding of Ni can further effectively reduce the dissolving of pad, and a part of Cu atom participates in and the interfacial reaction of Sn because Ni can replace, form (Cu, Ni)
6Sn
5The intermetallic compound of structure, the adding of Ni simultaneously also can reduce the bridging of the solder joint in the welding process; The interpolation of other trace elements can improve the oxidation resistance and the wettability of solder, and helps refinement solder joint crystal grain, improves the mechanical property of solder.
The alloy of being invented can adopt conventional method to make various solder products, comprises solder piece, welding rod, welding wire, soldered ball, weld-ring, weldering paper tinsel, welding powder or soldering paste.
Compared with prior art, the present invention has following remarkable result:
1, the fusion temperature of alloy of the present invention is higher and have good wettability, and melting range can substitute the high lead solder in the Electronic Packaging between 240～320 ℃, is used for the one-level encapsulation;
2, the present invention has added Cu and Ni on the basis of Sn-Sb alloy, has improved the melting behavior of solder effectively, and has significantly reduced the dissolution velocity of pad in solder under the high-temperature soldering condition, has increased the reliability of components and parts;
3, after the present invention has added micro-Ga, P and mishmetal in alloy, can make alloy under molten condition, have oxidation resistance preferably, and have the excellent wetting capacity energy.
The specific embodiment
Embodiment one
Alloy composition and percentage by weight thereof are: 12.38%Sb, and 4.47%Cu, 0.28%Ni, remaining is Sn and some common impurity elements.Measure by DSC, the melting range that draws alloy is: 246.2 ~ 292.3 ℃, tensile strength is 68.2MPa, sees Table 1 and table 2 respectively.
With diameter is that the Cu silk of 0.15mm is dipped in the molten solder and reacts, and investigates the corrode rate of alloy to the Cu matrix by measuring behind the immersed solder different time diameter of Cu silk.Experimental result shows that under 400 ℃ temperature, this alloy mainly occurs in the 2s the corrode behavior of Cu, and the corrode rate of Cu silk is 12.2%, and the Cu filament diameter is basicly stable behind the 2s, sees Table 1.
Preparation method of the present invention is: it is that the various alloying elements that will prepare are incubated 1～2h with vacuum melting furnace or non-vacuum melting stove down at 850～900 ℃, makes it even fusing, and fully stirs before coming out of the stove, and obtains solder behind the casting solidification.
Described solder is formed at least a in solder foundry alloy or solder piece or welding wire or soldered ball or weld-ring or weldering paper tinsel or welding powder or the soldering paste.
The described preparation method of present embodiment and following examples and above-mentioned basic identical, and can in said temperature and time range, select arbitrarily.
Embodiment two
Alloy composition and percentage by weight thereof are: 14.36%Sb, and 4.42%Cu, 0.28%Ni, remaining is Sn and some common impurity elements.The fusing point that DSC records is: 249.5 ~ 295.4 ℃, tensile strength is 71.3MPa.
This alloy mainly occurs in the 2s the corrode behavior of Cu, and the corrode rate of the Cu silk of 0.15mm is 12.2%, and the Cu filament diameter is basicly stable behind the 2s.
Embodiment three
By following composition and percentage by weight alloying: Sb18.72% thereof, Cu4.51%, Ni0.31%, all the other are pure Sn and common trace impurity.It is 250.6 ~ 305.1 ℃ that DSC records fusing point, and tensile strength is 83.1MPa.
The corrode of 400 ℃ of following Cu occurs in the 1s, the corrode rate of the Cu silk of 0.15mm is 11.6% at this moment, the Cu filament diameter increases to some extent between 1～2s, this mainly be since alloy element content increase more after, formed more irregular intermetallic compound in the interfacial reaction process, thereby measurement result has been produced influence.Molten alloy fluid level gauge face easily forms the oxide-film of one deck grey.
Embodiment four
Alloy composition and percentage by weight thereof: Sb13.92%, Cu4.2%, Ni0.6%, X0.002%, all the other are pure Sn and common trace impurity.The fusing point that DSC records this alloy is 239.6 ~ 284.8 ℃, and tensile strength is 73.2MPa.
Equally, because alloying level increases, the fusion speed experimental result of Cu silk is Cu filament diameter overstriking to some extent on the contrary behind the 1s, and this is because the result that a large amount of interface compound produces equally.
Because the adding of anti-oxidant element X (X is a kind of or several combination arbitrarily among Ga, P and the mishmetal), the non-oxidizability of this alloy is good, and the fusion liquid level is mirror-like.
Embodiment five
Alloy composition and percentage by weight thereof: Sb10.35%, Cu4.99%, Ni0.48%, all the other are pure Sn and common trace impurity.Fusing point is 239.8 ~ 303.5 ℃, and tensile strength is 78.5MPa.The Cu filament diameter tended towards stability after the corrode experiment showed 2s.
Embodiment six
Alloying component is: Sb9.96%, and Cu5.05%, all the other are pure Sn and common trace impurity.Fusing point is 242 ~ 305.7 ℃, and tensile strength is 75.4MPa.
Although in the corrode experiment behind the 3s Cu filament diameter stable, obviously owing to there is not the Ni element, this alloy to the corrode rate of Cu matrix than containing the big of Ni alloy among the above embodiment.
Embodiment seven
Alloying component is: 12.65%Sb, remaining is pure Sn and common trace impurity.It is 247.7 ℃～268.4 ℃ that DSC records fusing point, and tensile strength is 58.7MPa.
Molten Cu speed is very fast, and the corrode rate of the Cu silk of 0.150mm is 52.6% in the 3s, and the Cu silk that is immersed in the 5s in this alloy is all fused.Compare with all embodiment of front, this alloy is the most serious to the dissolution rate of Cu, is unfavorable for practical application.Alloy surface forms the very thin grey black oxide-film of one deck easily.
Embodiment eight
Be convenient to contrast, during tensile strength, corrode rate and the wettability of 95Pb-5Sn solder also all is listed in the table below.As can be seen from Table 2, the tensile strength of 95Pb-5Sn solder has only 23MPa, and by contrast, the tensile strength of the high-temp leadless solder among the present invention is generally higher.
From the corrode situation, because the interfacial reaction of novel lead-free alloy and Cu matrix is very fast, it is to big than 95Pb-5Sn of the corrosion of Cu matrix, but from table 1 also as can be seen, can usually improve this too fast unfavorable aspect of a pair of Cu matrix corrode by adding Ni unit.The raising of the alloying level particularly adding of Ni can effectively reduce the corrode degree of Cu matrix, and this is very favorable for the microwelding process.
From wettability, under identical scaling powder and same temperature, all than the weak point of high lead solder, the while wetting power is bigger than high Pb's for the wetting time of high-temp leadless solder, and this shows that the wettability of high-temp leadless alloy is better than high Pb solder.The concrete outcome of above embodiment is listed in table 1 successively, in table 2 and the table 3.
The fusing point of table 1 alloy and to the corrode rate of Cu silk
Illustrate: the green diameter of Cu silk is 0.15mm in Cu silk fusion experiment.The scaling powder that uses in the immersed solder process is WS-302 type water soluble flux.
Table 2 tensile strength of alloys
(experiment condition: rate of extension is 10
-3/ s)
The wettability of table 3 solder (scaling powder is a WS-302 type water soluble flux)
Claims (4)
1, a kind of leadless electronic brazing filler metal, this solder is made up of by following percentage by weight following alloying element: Sb:10～22%, Cu:1～8%, Ni:0.01～2%, X:0～0.01%, Sn surplus; Wherein X refers to zero kind, a kind of or any several combination in Ga, P and the mishmetal.
2, leadless electronic brazing filler metal according to claim 1 is characterized in that described solder fusing point between 240 ℃～320 ℃, tensile strength 58-84Mpa.
3, a kind of preparation method of lead-free brazing as claimed in claim 1 or 2, it is characterized in that: the various alloying elements that will prepare are incubated 1～2h with vacuum melting furnace or non-vacuum melting stove down at 850～900 ℃, make it even fusing, and before coming out of the stove, fully stir, obtain solder behind the casting solidification.
4, the preparation method of lead-free brazing according to claim 1 is characterized in that described solder is formed at least a in solder foundry alloy or solder piece or welding wire or soldered ball or weld-ring or weldering paper tinsel or welding powder or the soldering paste.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100611669A CN101239425A (en) | 2008-03-13 | 2008-03-13 | Leadless high-temperature electronic solder and preparation |
| PCT/CN2008/071959 WO2009111932A1 (en) | 2008-03-13 | 2008-08-12 | Lead-free high-temperature electronic solder and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100611669A CN101239425A (en) | 2008-03-13 | 2008-03-13 | Leadless high-temperature electronic solder and preparation |
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| CN101239425A true CN101239425A (en) | 2008-08-13 |
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|---|---|---|---|
| CNA2008100611669A Pending CN101239425A (en) | 2008-03-13 | 2008-03-13 | Leadless high-temperature electronic solder and preparation |
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| WO (1) | WO2009111932A1 (en) |
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| CN102430873A (en) * | 2011-10-26 | 2012-05-02 | 浙江亚通焊材有限公司 | Lead-free solder for high-temperature electronic packaging and preparation method thereof |
| CN102500948A (en) * | 2011-11-04 | 2012-06-20 | 浙江亚通焊材有限公司 | Lead-free high-temperature soft solder and preparation method thereof |
| CN102642098A (en) * | 2012-04-23 | 2012-08-22 | 浙江省冶金研究院有限公司 | High-temperature antioxidant lead-free welding rod for dip soldering of enameled wire |
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| CN106624434A (en) * | 2016-11-30 | 2017-05-10 | 安徽华众焊业有限公司 | Tin antimony solder alloy |
| CN107177752A (en) * | 2017-06-05 | 2017-09-19 | 雅拓莱焊接科技（惠州）有限公司 | A kind of inexpensive dystectic leadless welding alloy and preparation method thereof |
| CN107234361A (en) * | 2017-06-16 | 2017-10-10 | 东莞市锡达焊锡制品有限公司 | A kind of high temperature lead-free solder silk |
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| CN111843279A (en) * | 2020-07-22 | 2020-10-30 | 昆山市宏嘉焊锡制造有限公司 | High-temperature oxidation-resistant SnSbCu lead-free solder |
| CN114918574A (en) * | 2022-06-21 | 2022-08-19 | 浙江亚通焊材有限公司 | Tin-based composite solder and preparation method thereof |
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| JP2001284792A (en) * | 2000-03-30 | 2001-10-12 | Tanaka Electronics Ind Co Ltd | Solder material and method for manufacturing semiconductor device using the same |
| US20040241039A1 (en) * | 2000-10-27 | 2004-12-02 | H-Technologies Group | High temperature lead-free solder compositions |
| JP4147875B2 (en) * | 2002-09-19 | 2008-09-10 | 住友金属鉱山株式会社 | Brazing material, method of assembling semiconductor device using the same, and semiconductor device |
| JP4401671B2 (en) * | 2003-03-31 | 2010-01-20 | 千住金属工業株式会社 | High temperature lead-free solder alloys and electronic components |
| CN100467191C (en) * | 2005-10-28 | 2009-03-11 | 河南科技大学 | High-temp leadless soft solder |
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- 2008-08-12 WO PCT/CN2008/071959 patent/WO2009111932A1/en active Application Filing
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| CN102430873B (en) * | 2011-10-26 | 2015-06-03 | 浙江亚通焊材有限公司 | Pb-free solder for high-temperature electronic packaging and preparation method thereof |
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| CN115255710A (en) * | 2022-07-15 | 2022-11-01 | 郑州轻工业大学 | High-entropy alloy soft solder containing Sn and Cu and preparation method thereof |
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|---|---|
| WO2009111932A1 (en) | 2009-09-17 |
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Application publication date: 20080813 |