CN101092006A - Lead-free solder for micro alloyed eutectic alloy of stannum and zinc - Google Patents
Lead-free solder for micro alloyed eutectic alloy of stannum and zinc Download PDFInfo
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- CN101092006A CN101092006A CNA2006100893628A CN200610089362A CN101092006A CN 101092006 A CN101092006 A CN 101092006A CN A2006100893628 A CNA2006100893628 A CN A2006100893628A CN 200610089362 A CN200610089362 A CN 200610089362A CN 101092006 A CN101092006 A CN 101092006A
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Abstract
The invention discloses a micro-alloying tin-zinc eutectic alloy tinless solder that the main constituent is Sn-Zn eutectic alloy, Zn is 8-10wt% and the rest is Sn, adding one or the complex from Ga, P, Al, Ge, and Mg, the content of single alloy element is below 0.1%. The invention extremely maintains the feature of Sn-Zn eutectic alloy, and has the advantages of strong oxidation resistance, simple constituents, easy to recycle, etc.
Description
Technical field
The invention belongs to the special type function material field, relate to the leadless welding alloy in the welding field, specifically a class is applicable to the low-cost microalloying Sn-Zn of the anti-oxidant type eutectic alloy lead-free solder that microelectronics manufacturing and IC Packaging Industry are used.
Background technology
Along with the rise of " green welding " notion, the exploitation of novel lead-free solder has become the new problem that countries in the world solderer author faces.Why traditional tin-lead solder is used widely over the past thousands of years always is that performance excellent with it and cheap cost are inseparable, yet the toxicity of lead and lead compound causes people's attention day by day.Lead in the waste electronic product infiltrates soil after being dissolved in rainwater, directly influences human health by polluted source.Therefore forbid in recent years or limit and use the cry of lead more and more higher, and put into effect corresponding laws and regulations in succession and retrained, unprecedented pressure is generally felt in countries in the world, so the alternative existing Sn-Pb brazing filler metal alloy of development of new practicality electronics lead-free solder is extremely urgent.Although become the focus of field of functional materials in recent years at the research of electronics lead-free solder alloy, the lead-free solder alloy of having developed and declared patent is of a great variety, but these brazing filler metal alloys are compared with traditional Sn-Pb solder, the problem that has performance, technology or cost aspect does not more or less find gratifying Sn-Pb slicken solder substitute so far as yet.Desirable electronics lead-free solder alloy must have appropriate melting point, good wetability, favorable tissue stability, non-corrosiveness, and requires the raw material supply abundance, can satisfy the demand of industrialization etc.In binary or multicomponent alloy that current research is comparatively concentrated, Sn-Ag, Sn-Cu, Sn-Ag-Cu have the application of certain limit in the soldering industry, but the fusing point of these alloys is between 216-227 ℃, compare still higher with 183 ℃ of Sn-37Pb solder, the brazing temperature rising can make electronic component and baseplate material sustain damage, and a large amount of uses of Ag also are subjected to the restriction of resource aspect, it is estimated that the reserves of Ag will can not satisfy the huge market demand far away if all adopt the substitute of silver-containing solder as the Sn-Pb solder.
Make a general survey of candidate's alloy of numerous lead-free brazings, the tool temptation of Sn-9Zn eutectic alloy.The fusing point of this eutectic alloy is 199 ℃, very near the Sn-37Pb alloy melting point.With Sn-Zn is that the traditional Sn-Pb of alloy replacement is that alloy need not existing equipment is carried out big transformation, can continue to use the auxiliary material of original Sn-Pb brazing filler metal alloy soldering, and Sn-Zn is that cheap, the aboundresources of alloy also is that existing other lead-free solder alloy is incomparable.But the chemical property of Zn element is active, the surface film oxide that room temperature condition generates down is difficult to passivation, degree of oxidation aggravation under molten condition, give the melting of solder, preparation and welding bring a series of problems, this also is the principal element of this alloy of restriction in the extensive use of Electronic Packaging industry, therefore cause people's extensive concern in recent years at the research of Sn-Zn solder alloy, relevant research report and patent composition are constantly released, only domestic Sn-Zn base solder patent quantity open at present and that authorized is just multinomial near 20, the alloying element that adds mainly contains Ag, In, Bi, Ni, Sb, Cu, Al, Re etc., but from patent content, the characteristics that ubiquity alloying component complexity and composition range are wide in range, this has influence on the popularization of solder to application to a certain extent.So although the patent of Sn-Zn is more, but really can obtain to use and to obtain the Sn-Zn solder of customer acceptance still very few at present, use the more successful inner Sn-Zn-Al solder alloy of releasing of this Fuji Tsu of a few days still, this composition has obtained the United States Patent (USP) mandate, this solder alloy Al content is controlled at about 30PPm, belong to trace, in fact still belong to the Sn-Zn binary eutectic alloy.The improvement of this high performance-price ratio solder alloy successfully for the research and development of red brass solder provide can be for the thinking of using for reference, by adding the brazing property that anti-oxidant element, surface active element and easy passivation alloying element improve the Sn-9Zn alloy, become the major technique approach of practical Sn-Zn series lead-free solder exploitation.
Summary of the invention
Be difficult for removing the problems such as wetability difference that caused in order to solve Sn-9Zn the eutectic alloy easily oxidation of liquid alloy surface, oxide-film under non-vacuum condition, the object of the present invention is to provide a kind of performance, intact (antioxygenic property is good, wetting and spreading is good; Mechanical performance, electrical property are good), good, the service-strong lead-free solder for micro alloyed eutectic alloy of stannum and zinc of technology yield, this solder keeps the characteristics of Sn-Zn binary eutectic alloy to greatest extent, simultaneously overcome the adverse effect that grand alloying is brought alloy property, cost of alloy and soldering reliability aspect again, be convenient to promote to scolder manufacturing industry and Electronic Packaging field.
The objective of the invention is to reach by the following technical programs:
A kind of lead-free solder for micro alloyed eutectic alloy of stannum and zinc is characterized in that its alloy composition and content are by weight: Zn 8-10%; The micro alloying element that adds is a kind of or wherein several compound among Ga, P, Al, Ge, the Mg, and the upper content limit of its micro alloying element is 0.1 weight %, and surplus is Sn.
A kind of optimal technical scheme is characterized in that: also contain Cu, Ni, among the Ag one or more of trace in the described lead-free solder for micro alloyed eutectic alloy of stannum and zinc, its upper content limit 0.1 weight %.
Solder of the present invention can mix when reclaiming, and the different factor of micro alloying element can be ignored, and this recycling for control of the material composition in the scolder preparation process and scolder provides very big convenience.
The technical scheme of Sn-Zn base eutectic lead-free solder provided by the invention is on the basis of Sn-Zn binary eutectic alloy composition, in Ga, the Ge of interpolation trace, Mg, Al, the P alloying element one or more, the addition of trace element is below the 0.1 weight %, the interpolation element priority principle of selecting is the individual element microalloying, its priority is: Ga, P, Al, Ge, Mg, the selection of micro alloying element need be considered easily acquired, the scolder preparation technology and the soldering processes condition of raw material.Add separately the simplification of having guaranteed the brazing filler metal alloy composition, be easy to technology controlling and process, do not change other physical property of alloy simultaneously again.Micro alloying element can compound interpolation principle provide convenience for the recycling of scolder.Reclaiming solder can sort out respectively by micro alloying element, also can ignore the different influence of micro alloying element.The alloying element visual fusion point height that alloy of the present invention added can adopt pure simple substance element to add; also can adopt the intermediate alloy mode to add; the negative effect of as far as possible avoiding high melt that the alloy degree of purity is brought; the preparation of solder foundry alloy can be adopted common melting means; cooperate necessary safeguard measure, to improve the metallurgical quality of alloy.The determined micro alloying element of brazing filler metal alloy of the present invention all preferably comes out on a large amount of experiment basis, their effect comprises that surface or interface are poly-partially, reduces the liquid alloy surface tension, is difficult for oxidation or easily passivation, changes surface film oxide formation or structure, and by micro-solid solution or separate out the mechanical property that to improve brazing filler metal alloy in right amount, can improve the soldering reliability of solder to a certain extent.
Principle of the present invention is: the oxidation behavior result of study of Sn-Zn binary eutectic alloy under hot conditions shown that the oxidation of alloy at first is the oxidation of Zn, comprises ZnO
2, ZnO etc., secondly be the oxidation of Sn, oxidation product is SnO
2, SnO and Sn
3O
4Deng, the main body composition of oxide-film is the oxide of zinc, this oxide-film passivation ability a little less than, along with the prolongation of high-temperature residence time, oxidation weight gain curve keeps approximate linear rule.Based on above-mentioned result of study, know-why of the present invention is to add certain specific surface active element or micro-anti-oxidant element in alloy, make it gather surface partially by means of the reciprocation of these microalloy elements and alloy substrate at liquid alloy, form the surface enrichment layer of one deck enrichment, under hot conditions, the surface enrichment layer of this gathering trace element is difficult for oxidation or preferential oxidation, changed the skin covering of the surface characteristic, slowed down the further oxidation of liquid level, thereby reach the purpose that reduces the alloy surface oxidation rate, the wetting and spreading performance of liquid solder and substrate in the time of also will taking into account soldering when promoting surface passivation, avoid the interpolation of alloying element and the formation of passive oxidation film to bring capillary increase, oxide-film is easy to remove under the brazing flux effect during soldering.Therefore the selection principle of micro alloying element be its should not oxidation or preferential oxidation, formation be easy to passivation skin covering of the surface, strong surface or interface aggregate effect are arranged, to consider also in addition and the factors such as compatibility of parent metal that the experiment relatively alloying element of back screening is five kinds that propose in the invention claim.
Determined solder microalloying principle by a large amount of orthogonal experiments, the addition that is single trace element is no more than 0.1 weight %, some trace alloying element is very high at the enrichment degree on surface, is example with Ga, and content is inner 2000-3000 times in its superficial layer.Adding too much, form second phase or the harmful field trash easily, influence the physical property and the mechanical property of brazing filler metal alloy, so the micro alloying element addition upper limit of brazing filler metal alloy is defined as 0.1%, is based on above-mentioned factor.And the solder of the present invention that contains two or more micro alloying element mainly is to consider that actual production and manufacturing firm's solder reclaim or the needs of reuse repeatedly, is convenient to the popularization of this solder in application.
Consider the difference of Electronic Packaging industry surface mount baseplate material, alloy of the present invention can be according to the different suitably interpolations of the application conditions alloying element identical with the substrate principal component, as be no more than Cu, Ni, the Ag etc. of the trace of 0.1 weight %, with the wetability that improves scolder and stablize the solder joint composition.
Alloy of the present invention can be made various solder products with varying degrees with routine techniques, and as scolder foundry alloy, welding rod, welding wire, soldered ball, welding powder and soldering paste, its suitable application area comprises various solder industries, is specially adapted to microelectronics surface mount and encapsulation field.
Compared with prior art, the present invention has following significant advantage
1. the present invention adopts the microalloying principle on Sn-Zn binary eutectic alloy basis, farthest kept the Sn-Zn binary eutectic alloy as distinct advantages that solder application had, approaching as fusing point and Sn-37Pb alloy, the freezing range minimum, the increase of the cost of alloy of bringing almost can be ignored.
2. the micro alloying element kind determined of the present invention is preferably come out in a large amount of experimental results, and the interpolation of trace can obviously improve the oxidation resistance of alloy under molten condition, makes alloy have good brazing property under atmosphere and protective condition.
3. one of distinguishing feature of the present invention is except limiting the alloying element kind, more the element addition has been done clear and definite content and has limited, and dwindling of content range is easier to the stable of solder alloy performance, is convenient to large-scale production tissue and controlling of production process simultaneously.
4. alloy of the present invention is followed the principle that alloying component is oversimplified, and single adding is to guarantee the at utmost performance of element interaction; The principle of polynary compound interpolation provides very big convenience for the organization of production and the recycling of solder.
5. the preparation of alloy of the present invention can be adopted conventional melting mode, and low-melting-point metal (Ga) can add by the simple substance element form, and other metal (Al, P, Ge, Mg, Ag, Cu, Ni etc.) can adopt the intermediate alloy mode to add, to guarantee the metallurgical quality of alloy.
Solder alloy of the present invention can be used for being processed into various solder products with varying degrees, as scolder foundry alloy, welding rod, welding wire, soldered ball and welding powder, is applicable to the use of microelectronics Packaging industry.
The present invention is described in detail below by drawings and Examples.It should be understood that described embodiment only relates to the preferred embodiments of the invention, do not breaking away under the spirit and scope of the present invention situation that the changes and improvements of various compositions and content all are possible.
Description of drawings
Fig. 1 is that the embodiment of the invention 1,2 and comparative example's 1 gained solder bead constant temperature in 250 ℃ of air are placed 10min cooling rear surface state diagram;
Fig. 2 is the embodiment of the invention 5 and Comparative Examples 1 scolder solder joint shape appearance figure;
Fig. 3 is the embodiment of the invention and comparative example's 1 gained brazing filler metal alloy constant temperature heat of oxidation weight analysis curve in 250 ℃ of air;
Fig. 4 is product form and preparation technology's flow chart thereof of lead-free solder for micro alloyed eutectic alloy of stannum and zinc of the present invention.
The specific embodiment
The melting of brazing filler metal alloy of the present invention and preparation technology specify.
Sn, Zn, Ga adopt the simple metal mode to add, Ge, Al, P, Ni adopt the intermediate alloy mode to add, and promptly adopt vaccum sensitive stove to smelt Sn-10Ge, Sn-10Al, Sn-5Ni and Sn-5P intermediate alloy (also can adopt quartz ampoule vacuum seal to place chamber type electric resistance furnace melting preparation) respectively.
Embodiment 1
With ready Sn, Zn, Sn-10Ge metal and alloy raw material; press Sn-8.8Zn-0.08Ge component prescription alloyage material 500g; utilize under the resistance furnace argon shield condition and carry out alloy melting; the alloy addition sequence is Sn, Zn, Sn-10Ge; the all molten clear back of alloy keeps 30min at 400 ℃; to guarantee the uniformity of composition, reduce heating power, treat that the solder melt temperature reduces to 250 ℃ and begin to be poured in the stainless steel steel mold of preheating.
Embodiment 8
With ready Sn; Zn; Ga; Sn-10Ge; Sn-10Al; Sn-5Ni and Sn-5P metal and alloy raw material; press Sn-8.7Zn-0.03Ga--0.015Ge-0.01Al-0.006P-0.04Ni component prescription alloyage material 500g; utilize under the resistance furnace argon shield condition and carry out alloy melting; the alloy addition sequence is Sn; Zn; Sn-10Ge; Sn-5Ni; Sn-10Al; Sn-5P; Ga; the all molten clear back of alloy keeps 30min at 400 ℃; to guarantee the uniformity of composition; reduce heating power, treat that the solder melt temperature reduces to 250 ℃ and begin to be poured in the stainless steel steel mold of preheating.
Other embodiment uses with the comparative example and prepares with the foregoing description 1 mode identical with 8, and its chemical composition sees Table 1.
Alloy of the present invention can be prepared into foundry alloy blank, welding rod, welding wire, soldered ball and welding powder, and concrete preparation technology sees accompanying drawing 4.Can adopt the simple metal mode to add, be about to simple metal raw material (comprising simple substance P) adding resistance furnace smelting furnace and prepare foundry alloy, perhaps adopt the intermediate alloy mode to add: promptly adopt vaccum sensitive stove or quartzy vacuum seal to place the chamber type electric resistance furnace melting to prepare intermediate alloy, and then adding resistance furnace smelting furnace to prepare foundry alloy; Then or by the powder process of ultrasonic atomizatio method; Perhaps be equipped with welding rod by the jet breakup legal system; Perhaps, pass through extruding again and draw welding rod and welding wire by metal pattern casting cast preparation casting welding rod.
Chemical composition of embodiment of the invention alloy and comparative example's alloy (weight %) and performance test results see the following form 1.
The chemical composition (weight %) and the performance test results of table 1, the embodiment of the invention and comparative example's alloy
| Brazing filler metal alloy | Zn | Ga | P | Al | Ge | Mg | Ag Cu Ni | Sn | 250 ℃ of test temperatures | ||
| 10min rear surface degree of oxidation * | Cu substrate spreading area/mm 2 | ||||||||||
| Embodiment | 1 | 8.8 | 0.08 | Surplus | 1 | 58.8 | |||||
| 2 | 9.2 | 0.08 | Surplus | 2 | 57.5 | ||||||
| 3 | 8.7 | 0.01 | Surplus | 2 | 54.6 | ||||||
| 4 | 8.7 | 0.01 | Surplus | 2 | 55.0 | ||||||
| 5 | 9.2 | 0.04 | Surplus | 2 | 56.0 | ||||||
| 6 | 8.7 | 0.03 | 0.02 | 0.07Ag | Surplus | 1 | 58.6 | ||||
| 7 | 9.0 | 0.005 | 0.01 | 0.06Cu | Surplus | 2 | 56.4 | ||||
| 8 | 8.7 | 0.03 | 0.006 | 0.01 | 0.015 | 0.04Ni | Surplus | 1 | 60.8 | ||
| The comparative example | 1 | 8.8 | |
3 | 49.4 | ||||||
| 2 | 9.1 | |
3 | 47.5 | |||||||
* annotate: the 1-surface-brightening; 2-surface is dim, slight oxidation is arranged; 3-surface blackening, oxidation are serious.
Brazing filler metal alloy high-temperature oxydation degree observation experiment method of the present invention:
As shown in Figure 1, constant temperature in 250 ℃ of air is placed 10min cooling rear surface state diagram for the embodiment of the invention 1,2 and comparative example's 1 gained solder bead.
(precision 0.1mg) takes by weighing the 0.3g solder alloy with electronic balance, and the quick oil quenching of heat fused and warp is prepared into bead in rosin liquid.Because the whole cooling procedure of solder bead is finished in rosin liquid and oil, so ignore the oxidation (in addition, all samples is not all considered the normal temperature solid oxide between the sample storage life) in the solder cooling procedure.Cooled solder globules dries up after acetone and the cleaning of alcohol ultrasonic wave.Under 250 ℃ of conditions, the solder bead is put on the corundum thin slice, the corundum thin slice is placed heat tracing on the heating plate of controllable temperature together with the solder bead, observe fusing solder bead in the change color of different heating under the time, and with digital camera Taking Pictures recording closely in real time, heat after 10 minutes the corundum thin slice taken out and be placed on cooling fast on the chill, by the relatively color on solder bead surface and the high-temperature oxidation resistance (see figure 1) that brightness changes the qualitative evaluation brazing filler metal alloy.As shown in Figure 1: the embodiment of the invention 1 gained solder bead surface-brightening, embodiment 2 gained solder beads surfaces is dim, slight oxidation is arranged, and comparative example's 1 gained bead surface blackening, oxidation are serious.In table 1, be expressed as follows respectively: the 1-surface-brightening; 2-surface is dim, slight oxidation is arranged; 3-surface blackening, oxidation are serious.
The wetting and spreading performance test of brazing filler metal alloy of the present invention:
As shown in Figure 2, be the solder joint shape appearance figure of the embodiment of the invention 5 brazing filler metal alloys and comparative example's 1 alloy.
According to Japanese JIS standard the 0.2+0.001g scolder being placed on purity is on 99.9% the copper plate, is incubated 90s on 250 ℃ of thermostatic electrothermal plates, and the cooling back is taken with digital camera.Before the experiment, copper coin sand paper fine grinding is cleaned with acetone and is removed greasy dirt and dip 5s removal surface film oxide in 10%HCl, fully washes with deionized water again, and the synthetic colophony type scaling powder of the CR22LU type of be sure oing Ai Fa company is adopted in this test.The solder joint area utilizes computer image treatment software to carry out accurate Calculation, and experimental result is the mean value of three experiments.Can find out obviously that scolder of the present invention compares spreading area with SnZn binary eutectic scolder and increase to some extent.Can illustrate that lead-free solder spreading property of the present invention is good, have higher solderability from the full degree of the rounding on solder joint surface.
Thermogravimetric (TGA) contrast test
As shown in Figure 3, be respectively embodiment of the invention 1-7 and the thermogravimetric analysis curve of comparative example's 1 brazing filler metal alloy under 250 ℃.
This experiment is cut into square and almost spherical with solder, and weight is fixed on about 0.1g, and the solder fritter is inserted in the oxidation crucible.Instrument model STA409PC; Sensitivity :≤0.1 μ g; Atmosphere: air.Programming rate: 10 ℃/min; Thermostat temperature: 250 ℃; Temperature retention time: 25min.The oxidation rate of solder is shown with the mass change of per surface area, considers that solder is placed in the corundum crucible, so can trend towards sphere after the fusing of solder piece, calculates by spherical so surface area of sample is approximate.Test result shows that the oxidation weight gain speed of solder of the present invention is starkly lower than the comparative example, and this quantitative result reflects that solder of the present invention has good high temperature oxidation resistance.
Claims (2)
1, a kind of lead-free solder for micro alloyed eutectic alloy of stannum and zinc is characterized in that its alloy composition and content are by weight: Zn 8-10%; The micro alloying element that adds is a kind of or wherein several compound among Ga, P, Al, Ge, the Mg, and the upper content limit of its micro alloying element is 0.1%, and surplus is Sn.
2, lead-free solder for micro alloyed eutectic alloy of stannum and zinc according to claim 1 is characterized in that: also contain Cu, Ni, among the Ag one or more of trace in the described lead-free solder for micro alloyed eutectic alloy of stannum and zinc, its upper content limit 0.1 weight %.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100893628A CN101092006A (en) | 2006-06-21 | 2006-06-21 | Lead-free solder for micro alloyed eutectic alloy of stannum and zinc |
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|---|---|---|---|
| CNA2006100893628A CN101092006A (en) | 2006-06-21 | 2006-06-21 | Lead-free solder for micro alloyed eutectic alloy of stannum and zinc |
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| CN101092006A true CN101092006A (en) | 2007-12-26 |
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| JPWO2021010199A1 (en) * | 2019-07-12 | 2021-01-21 | ||
| CN114206542A (en) * | 2019-07-12 | 2022-03-18 | 亚特比目有限会社 | SnZn solder and manufacturing method thereof |
| CN111085799A (en) * | 2020-01-19 | 2020-05-01 | 上海锡喜材料科技有限公司 | Formula of soft soldering wire product without flux core for TC power device |
| WO2021256172A1 (en) * | 2020-06-16 | 2021-12-23 | アートビーム有限会社 | Snzn solder and production method therefor |
| CN112404791A (en) * | 2020-11-18 | 2021-02-26 | 昆明理工大学 | Tin-zinc series lead-free solder alloy and preparation method thereof |
| CN115383344A (en) * | 2022-06-06 | 2022-11-25 | 桂林航天工业学院 | In-48Sn-xCuZnAl composite solder and preparation method and application thereof |
| CN115383344B (en) * | 2022-06-06 | 2024-02-06 | 桂林航天工业学院 | In-48Sn-xCuZnAl composite solder and preparation method and application thereof |
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