CN101381826B - Sn-Cu base leadless solder alloy and preparation method - Google Patents
Sn-Cu base leadless solder alloy and preparation method Download PDFInfo
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Abstract
The invention relates to tin-copper-based lead-free solder alloy and a preparation method thereof. The compositions in mass percentage of the alloy are 0.1 to 1.5 percent of copper, 0.001 to 1 percent of phosphor, 0 to 6 percent of bismuth, 0 to 3 percent of zinc, and the balance being tin. The preparation method comprises the following steps: 3 to 8 percent of the phosphor and 92 to 97 percent of the tin are weighed at first and placed into a graphite crucible; the mixture is covered with protective molten salt and subjected to heat preservation for 30 to 60 minutes at a temperature of between 400 and 550 DEG C; after uniform stirring, casting is performed and tin-copper intermediate alloy is obtained; the tin-copper intermediate alloy is weighed according to the fact that the phosphor occupies 0.001 to 1 percent as calculated by the total mass of 100 percent, and 0.1 to 1.5 percent of the copper, 0 to 6 percent of the bismuth, 0 to 3 percent of the zinc and residual tin are weighed and placed into the graphite crucible; the mixture is covered with the protective molten salt and subjected to heat preservation for 40 to 80 minutes at a temperature of between 450 and 550 DEG C; and after uniform stirring, the mixture is cast into ingots. The preparation method has simple preparation technique and is easy to operate; and the product of the tin-copper-based lead-free solder alloy has the advantages of good wettability, low melting point, good mechanical property, good antioxidation, low cost and so on.
Description
Technical field:
The invention belongs to the non-ferrous alloy material, what relate to is a kind of unleaded brazing material, specially refers to a kind of Sn-Cu base leadless solder alloy that the electronic component soldering is used and preparation method thereof that is applicable to.
Background technology:
Sn-Pb eutectic and nearly eutectic alloy because cheap, fusing point is low, advantages such as the wetability of copper base is good are obtained extensive use in electronics industry.Enhancing along with human environmental consciousness; Lead and compound thereof cause global showing great attention to the harmfulness of environment and human health; International community has put into effect a series of regulation limitations in succession or has forbidden containing the use of Pb solder, and the lead-free brazing of development function admirable, environmental protection is imperative.
Countries in the world have been carried out big quantity research in recent years, have developed multiple lead-free solder alloy, are broadly divided into binary alloy systems such as Sn-Ag, Sn-Cu, Sn-Bi and Sn-Zn, and add ternary, quaternary alloy system that the 3rd, the 4th constituent element forms on this basis.But do not find all gratifying Sn-Pb solder of various aspects of performance substitute so far as yet.The wherein wetability and the corrosion resistance extreme difference of Sn-Zn system; The fusing point of Sn-Bi also possibly make solder produce fragility far below Sn-Pb and Bi; The performance of having generally acknowledged at present relatively better, what be applied in some occasions is Sn-Ag and Sn-Ag-Cu alloy; But the fusing point of Sn-Ag and Sn-Ag-Cu alloy (about 220 ℃) is too high with respect to existing Sn-Pb eutectic alloy solder fusing point (183 ℃), be difficult to and existing circuit sheet material, electronics soldering production technology and hardware compatibility, and cost of material is also higher.Sn-Cu is that the primary raw material Sn of alloy, the reserves of Cu enrich; Cheap; The cost of most of lead-free brazings is than the high 2-3 of Sn-Pb solder times, and the Sn-0.7Cu alloy is only high 1.3 times than Sn-Pb solder by contrast, is one of solder that cost is minimum relatively in the lead-free brazing of being studied at present; This alloy also has and has no side effect, and is prone to produce, is prone to advantages such as recovery, and Sn-Cu is one of alloy product of becoming the most potential alternative Sn-Pb solder.But the eutectic temperature of this bianry alloy (227 ℃) is higher; Non-oxidizability, corrosion resistance are relatively poor, and comprehensive mechanical property is relatively poor, and the wetability of Sn-Cu lead-free brazing on the Cu base is not ideal enough simultaneously; These shortcomings have limited the use of this alloy greatly; The Sn-Cu alloy has mainly obtained application in wave-soldering technology at present, because fusing point is too high, in reflow soldering process, does not almost obtain to use.
Summary of the invention
The objective of the invention is; To the problems referred to above that exist in the Sn-Cu alloy, improve the mechanical property of Sn-Cu alloy, non-oxidizability and corrosion resistance through adding an amount of alloy constituent element; And can significantly improve the wetability of this alloy on copper; The fusing point of this alloy is effectively reduced, the new formulation of the Sn-Cu base leadless solder alloy of, high comprehensive performance cheap to obtain to have, and this kind Sn-Cu is provided the preparation method of base leadless solder alloy.
Sn-Cu base leadless solder alloy of the present invention, its Cu content are the 0.1-1.5% of alloy gross weight, and P content is the 0.001-1% of alloy gross weight, and Bi content is the 0-6% of alloy gross weight, and Zn content is the 0-3% of alloy gross weight, and surplus is Sn.
More excellent technical scheme of the present invention is: its Cu content is the 0.1-1.5% of alloy gross weight, and Bi content is the 0.1-6% of alloy gross weight, and Zn content is the 0.1-3% of alloy gross weight, and P content is the 0.001-1% of alloy gross weight, and surplus is Sn.
Preparation method of the present invention is following:
1, take by weighing P 3～8% by mass ratio, Sn 92-97% puts into graphite crucible with both then; The covering protection fused salt places smelting furnace with crucible in the above, is incubated 30～60 minutes under 400～550 ℃ the temperature; Casting after stirring gets the Sn-P intermediate alloy;
2, be 100% by gross mass, the amount that accounts for 0.001-1% in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu0.1-1.5% again; Bi 0-6%, Zn 0-3%, surplus is Sn; Batching is put into graphite crucible, and the covering protection fused salt places smelting furnace with crucible above that; Be incubated 40～80 minutes under the 450-550 ℃ of temperature, be cast into ingot after stirring, promptly get required brazing filler metal alloy.
Protection fused salt of the present invention can be the mixture of KCl and LiCl, also can be the mixture of LiCl and LiF or NaCl, and the melting range of used protection fused salt is generally selected between 300～500 ℃.
When protection fused salt according to the invention was got the mixture of KCl and LiCl, can be with KCl, LiCl with (1.2～1.5): the mass ratio of (0.9～1.1) mixes, dry and get final product.
The present invention is to provide that a kind of wetability is good, fusing point is lower, good mechanical properties, the low-cost preferably lead-free solder alloy of non-oxidizability, add antioxygenic property, corrosion resistance and the wettability on the Cu base thereof that P can significantly improve alloy; Add a spot of Bi and can improve the wettability of alloy on Cu to a certain extent, and reduce the fusing point of this alloy; Interpolation Zn helps improving the mechanical performance of alloy, and is also useful to the welding spot reliability that improves alloy and Cu formation.Adopt Cu surface spreading wetting experiment to weigh the wetability of alloy on Cu; Find that the simple Sn-Cu alloy wetability of Sn-Cu alloy ratio of adding a small amount of P or Bi significantly improves; Basically can reach the level of Sn-Pb alloy, and be higher than the Sn-Ag (Cu) wetability of alloy; Add Bi the fusing point of Sn-Cu alloy is significantly reduced, make its fusing point can reach the level that Sn-Ag is an alloy at least, this helps promoting the application of Sn-Cu alloy in reflow soldering process; Be higher than the Sn-Pb brazing filler metal alloy even its intensity is approaching, thereby long service life and higher reliability are arranged.With respect to other Sn-Cu solder alloys that adds dystectic Ni, the present invention adds P, Bi, Zn, and additive material is bought on market easily, does not adopt precious metal, makes its cost more cheap, and preparation technology is simple, and operation has good development potentiality easily.Comprehensive considering various effects, the present invention has cost performance and practicality preferably.
Description of drawings
Fig. 1 is the spreading area of Sn-0.7Cu brazing filler metal alloy on Cu of different P additions.
Fig. 2 is the influence of adding P to Sn-0.7Cu brazing filler metal alloy non-oxidizability at 260 ℃.
Fig. 3 is for adding Bi and the P influence to Sn-0.7Cu brazing filler metal alloy wetability on Cu.
Specific embodiment
The present invention will do explanation further through following examples.
The used protection fused salt of following examples is with KCl: LiCl mixes, dries gained with 1.3: 1 mass ratio.
Embodiment 1:
1, take by weighing P 4% by mass ratio, Sn 96%, is 50 grams altogether; Then both are put into graphite crucible, and cover the above-mentioned molten fused salt for preparing in the above, crucible is placed resistance furnace; Temperature is 450 ℃ and is incubated 45 minutes down that the back casting that stirs gets the Sn-P intermediate alloy;
2, be 100% by gross mass, 0.1% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 0.7% again, and surplus is Sn, and gross weight is 100 grams.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed resistance furnace, insulation is 60 minutes under 450 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
Molten as stated above Sn-Cu alloy of having joined a series of different P content supplies wetability and non-oxidizability to measure; The brazing filler metal alloy of different P content is seen accompanying drawing 1 to the influence of Cu wetability.P content is seen accompanying drawing 2 to the influence of brazing filler metal alloy non-oxidizability.
Wetability is weighed through the spreading area of brazing filler metal alloy on the copper base.Measuring method is: with diameter is that the 0.3g brazing filler metal alloy disk of 8mm places the copper sheet central authorities that covered one deck scaling powder (RMA), have been of a size of 40mm * 40mm * 0.1mm; Again at the same autogamy scaling powder of surface coverage one deck of brazing filler metal alloy; It is placed reflow soldering, and 250 ℃ of refluxed 15 seconds, sample was taken out in the cooling back; Photograph it with digital camera and on copper sheet, sprawl the plane, calculate the brazing filler metal alloy spreading area through Image Pro Plus image analysis software; Measure 5 times, get the measurement result of its mean value as spreading area.Accompanying drawing 1 has provided the gained result.Wherein content is the wetability level that 0 point is represented the Sn-0.7Cu mother metal.The result shows that several kinds of alloy wetabilitys of adding trace P all are significantly increased with respect to pure Sn-0.7Cu alloy.
Weigh the non-oxidizability of each brazing filler metal alloy with the weightening finish method.Fig. 2 has provided measurement result.As can be seen from the figure, under equal conditions, add P the weightening finish of alloy on unit are reduced, promptly the non-oxidizability of alloy is significantly improved.
Embodiment 2:
1, take by weighing P 4% by mass ratio, Sn 96%, is 50 grams altogether; Then both are put into graphite crucible, and cover the above-mentioned molten fused salt for preparing in the above, crucible is placed induction furnace; Be 500 ℃ in temperature and be incubated 30 minutes down that the back casting that stirs gets the Sn-P intermediate alloy;
2, be 100% by gross mass, 0.05% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 0.7% again, and P 0.05%, and Bi 1%, and surplus is Sn, and gross weight is 100 grams.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed induction furnace, insulation is 30 minutes under 500 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
Molten as stated above Sn-0.7Cu base alloy of having joined a series of different B i content and P content supplies wetability and fusing point to measure.Each alloy characterizes with its spreading area on the Cu surface the wetability of Cu.The method that is adopted among measuring method and the embodiment 1 is identical.Accompanying drawing 3 and subordinate list 1 have provided the measurement result of wetability and fusing point respectively.The result shows: add a small amount of Bi or add Bi simultaneously, P has raising by a relatively large margin to the wetability of alloy; Add the fusing point that Bi or P can reduce the Sn-0.7Cu brazing filler metal alloy simultaneously, make its fusing point can be reduced to Sn-Ag (level Cu) at least.
Embodiment 3:
1, take by weighing P 4% by mass ratio, Sn 96%, is 50 grams altogether; Then both are put into graphite crucible, and cover the above-mentioned molten fused salt for preparing in the above, crucible is placed induction furnace; Temperature is 400 ℃ and is incubated 60 minutes down that the back casting that stirs gets the Sn-P intermediate alloy;
2, be 100% by gross mass, 0.05% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 0.7% again, and P 0.05%, and Bi 1%, and Zn 1%, and surplus is Sn, and gross weight is 100 grams.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed induction furnace, insulation is 30 minutes under 500 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
The molten as stated above Sn-0.7Cu-1Bi-1Zn that has joined a series of P content is an alloy, supplies wetability to measure.Each alloy characterizes with its spreading area on the Cu surface the wetability of Cu.The method that is adopted among measuring method and the embodiment 1 is identical.The result shows: adding a small amount of P all has raising by a relatively large margin to the wetability of alloy.
Embodiment 4:
1, take by weighing P 3% by mass ratio, Sn 97%, and both are put into graphite crucible, and covers the above-mentioned fused salt for preparing that melts in the above, and crucible is placed resistance furnace, and temperature is 550 ℃ and is incubated 30 minutes down that the back casting that stirs gets the Sn-P intermediate alloy;
2, be 100% by gross mass, 1% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 1.5% again, and surplus is Sn.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed resistance furnace, insulation is 60 minutes under 450 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
Embodiment 5:
1, take by weighing P 8% by mass ratio, Sn 92%, and both are put into graphite crucible, and covers the above-mentioned fused salt for preparing that melts in the above, and crucible is placed induction furnace, is 450 ℃ in temperature and is incubated 45 minutes down, and the back casting that stirs gets the Sn-P intermediate alloy;
2, be 100% by gross mass, 0.002% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 0.1% again, and Bi 0.8%, and surplus is Sn.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed induction furnace, insulation is 30 minutes under 500 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
Embodiment 6:
1, take by weighing P 5% by mass ratio, Sn 95%, and both are put into graphite crucible, and covers the above-mentioned fused salt for preparing that melts in the above, and crucible is placed induction furnace, is 450 ℃ in temperature and is incubated 45 minutes down, and the back casting that stirs gets the Sn-P intermediate alloy;
2, by gross mass 100%, 0.05% the amount of accounting in P takes by weighing the Sn-P intermediate alloy, takes by weighing Cu 0.7% again, and Bi 1%, and Zn 1%, and surplus is Sn.Batching is put into graphite crucible, cover above-mentioned protection fused salt above that, crucible is placed induction furnace, insulation is 30 minutes under 500 ℃ of temperature, is cast into ingot after stirring, and promptly obtains required brazing filler metal alloy.
Following table is that the present invention adds Bi or the P influence to Sn-0.7Cu brazing filler metal alloy fusing point.
Claims (1)
1. a Sn-Cu base leadless solder is characterized in that Cu content is the 0.1-1.5% of alloy gross weight, and Bi content is the 0.1-6% of alloy gross weight, and Zn content is the 0.1-3% of alloy gross weight, and P content is 0.1%＜P≤1% for the alloy gross weight, and surplus is Sn; Its preparation process is:
(1) take by weighing P 3～8% by mass ratio, Sn 92-97% puts into graphite crucible with both then; The covering protection fused salt places smelting furnace with crucible in the above, is incubated 30～60 minutes under 400～550 ℃ the temperature; Casting after stirring gets the Sn-P intermediate alloy;
(2) be 100% by gross mass, take by weighing the Sn-P intermediate alloy, take by weighing Cu 0.1-1.5% again in the amount of 0.1%＜P≤1%; Bi 0.1-6%, Zn 0.1-3%, surplus is Sn; Batching is put into graphite crucible, and the covering protection fused salt places smelting furnace with crucible above that; Be incubated 40～80 minutes under the 450-550 ℃ of temperature, be cast into ingot after stirring, promptly get required brazing filler metal alloy.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI602928B (en) * | 2015-11-30 | 2017-10-21 | 千住金屬工業股份有限公司 | Solder alloy |
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| CN101780607B (en) * | 2010-03-17 | 2012-05-09 | 华南理工大学 | Lead-free solder for electronic packaging, assembling and soldering and preparation method thereof |
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