CN101885119B - Sn-Cu-Ni lead-free solder containing V, Nd and Ge - Google Patents
Sn-Cu-Ni lead-free solder containing V, Nd and Ge Download PDFInfo
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- CN101885119B CN101885119B CN2010102169054A CN201010216905A CN101885119B CN 101885119 B CN101885119 B CN 101885119B CN 2010102169054 A CN2010102169054 A CN 2010102169054A CN 201010216905 A CN201010216905 A CN 201010216905A CN 101885119 B CN101885119 B CN 101885119B
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Abstract
The invention relates to Sn-Cu-Ni lead-free solder containing V, Nd and Ge, belonging to metal materials and brazing materials in the metallurgical field. The Sn-Cu-Ni lead-free solder containing V, Nd and Ge comprises the following chemical compositions in percentage by weight: 0.07-1.8 percent of Cu, 0.01-2.0 percent of Ni, 0.001-0.1 percent of V, 0.001-0.4 percent of Nd, 0.001-0.1 percent of Ge and the balance of Sn. The invention has the advantages that the Sn-Cu-Ni lead-free solder has improved wettability, thermal stability of internal texture in a service process, mechanical performance of welding points, fatigue resistance, guaranteed content accuracy of trace element Nd in solder, excellent processing performance, stronger oxidation resistance capability, even soldering seam fine texture, favorable wettability, excellent mechanical performance of soldering seam and greatly improved fatigue resistance of joints, can satisfy the lead-free requirement of an RoH instruction and the need for environment-friendly manufacture and can be suitable for the needs of different production conditions.
Description
Technical field
The present invention relates to the Sn-Cu-Ni lead-free brazing of a kind of V of containing, Nd and Ge, belong to the brazing material of class of metal materials and field of metallurgy.Be mainly used in surface-assembled and encapsulation field, to satisfy the needs of green manufacturing.
Background technology
On July 1st, 2006; Since the RoHS of European Union (The Restriction of the Use of certain Hazardous Substance in Electrical and Electronic Equipment) instruction was formally effective, the substitution problem of tin-lead solder became the hot subject of electron trade technical staff research.Though Sn-Cu-Ni brazing filler metal low price, cost are merely 1.3 times of the plumbous eutectic solder of tin, wettability is compared with tin-lead solder and is still had a certain distance.Sn-Cu-Ni solder cost has greater advantage than the Sn-Ag-Cu brazing filler metal alloy; Be prone to produce and reclaim; And electronic product there is reasonable compatibility and receives electron trade users' favor; Have a good application prospect [Chinese patent ZL99800339.5], but still also there are many deficiencies in the Sn-Cu-Ni solder, has limited its application in welding procedures such as reflow welding.The researcher is mainly through adding some trace elements at present; Come further to optimize the performance of Sn-Cu-Ni brazing filler metal through microalloying; The publication achievement that some correlative studys also occurred, achievement in research mainly is usually to optimize the performance that Sn-Cu-Ni is a solder alloy through adding units such as Sb, P, rare earth element ce both at home and abroad.Japan Nihon Superior Co., Ltd. has researched and developed the Sn-Cu-Ni lead-free brazing, and trade name is SN100C, and has obtained this patent in 24 countries and regions that comprise Japan, the U.S. and China; The patent of optimizing the Sn-Cu-Ni solder performance through the adding rare earth element mainly concentrates on China, the main Sn-of representational publication achievement (0.8-3.0wt.%) Cu-(0.01-1.6wt.%) Ni-(0.005-0.2wt.%) Pb-(0.001-0.1wt.%) Ce [patent ZL 200510022563.1] etc.Since also have many technical problems for example the uniformity or the like of wetting and spreading property, mechanical property, oxidation resistance and brazed seam microstructure need badly new achievement in research come perfect, replenish this invention " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " i.e. completion under this technical background.
Summary of the invention
The object of the present invention is to provide and a kind ofly help to remedy the shortcoming and defect of Sn-Cu-Ni solder and use the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge that embodies that wetting and spreading property is good, mechanical property is excellent and cost is cheap relatively and can satisfy the green manufacturing needs of product.
For reaching the foregoing invention purpose; The technical scheme that this invention provides is: the Sn-Cu-Ni lead-free brazing of a kind of V of containing, Nd and Ge, and its chemical composition by the mass percent proportioning is: 0.07～1.8% Cu, 0.01～2.0% Ni; 0.001～0.1% V; 0.001～0.4% Nd, 0.001～0.1% Ge, surplus is Sn.
The technique effect of technical scheme provided by the invention is: polynary compound interpolation trace element V, rare earth Nd and Ge element and improve heat endurance, solder joint mechanical property and the fatigue resistance of interior tissue in Sn-Cu-Ni series leadless solder wettability, the military service process through its acting in conjunction in the Sn-Cu-Ni series leadless solder; Because the very easily oxidation of metal Nd element is prone to scaling loss during high temperature, therefore the form with intermediate alloy Sn-Nd adds to guarantee the accuracy of micro-Nd composition in solder; The brazing filler metal alloy that obtains has that superior processing characteristics, oxidation resistant ability are strong, the brazed seam microstructure is even, wettability good, brazed seam good mechanical performance and joint anti-fatigue performance significantly improve; Remedied some shortcoming and defect of Sn-Cu-Ni solder, combination property approaches the Sn-Pb solder; Can satisfy the needs of RoHS instruction to unleaded requirement and green manufacturing; Owing to have a superior processing characteristics, therefore can be processed into such as different shape such as strip, bar-shaped, thread and soldered ball and use the needs that adapt to different working conditions.
Description of drawings
Fig. 1 a is the sketch map of four limit flat package devices (Quad Flat Package is called for short QFP) the solder joint tensile force of different Nd content.
Fig. 1 b is the sketch map of the plate resistor solder joint shearing resistance of different Nd content.
Fig. 2 is the spreading area sketch map of heterogeneity brazing filler metal alloy.
Fig. 3 is same test conditions following fatigue life of the frequency diagram of heterogeneity brazing filler metal alloy.
Fig. 4 is the metallographic microstructure photo that does not add the Sn-Cu-Ni lead-free solder alloy of V, Ge and rare earth Nd.
Fig. 5 is the metallographic microstructure photo of the Sn-Cu-Ni lead-free solder alloy of interpolation V, Ge and rare earth Nd 0.05wt.%.
Fig. 6 is the metallographic microstructure photo of the Sn-Cu-Ni lead-free solder alloy of interpolation V, Ge and rare earth Nd 0.4wt.%.
Fig. 7 a is not for adding the unleaded welding point interface microstructure picture of Sn-Cu-Ni of V, Ge and rare earth Nd.
Fig. 7 b is for adding the unleaded welding point interface microstructure picture of Sn-Cu-Ni of V, Ge and rare earth Nd 0.4wt.%.
The specific embodiment
Adopt conventional method to prepare solder; Promptly use commercially available tin slab, cathode copper, metallic nickel, vanadium metal, germanium metal, neodymium metal; Various raw metals are proportioning on demand; Add during smelting through optimizing screening definite " coverture " or adopting " inert gas " protection to smelt, cast, can obtain bar.Through extruding, drawing, promptly obtain a material (also can add scaling powder, process " flux-cored wire ").Plumbous (being Pb) element is as " impurity element " in the raw material such as tin slab, cathode copper; Overall control (is stipulated Pb≤0.1wt.%) to satisfy the regulation meet State Standard of the People's Republic of China GB/T 20422-2006 " lead-free brazing " in the standard in 0.001～0.1% scope.
The present invention has mainly solved following two critical technical problems:
1) adopts the rare earth elemental metals neodymium; Add during smelting through optimizing " coverture " that screening confirms or the metallic tin that adopts " inert gas " to protect or adopt interpolation to smelt in advance and smelt with the method for the Sn-Nd intermediate alloy of rare earth elemental metals neodymium formation; Significantly reduced the scaling loss of rare earth elemental metals neodymium in melting and process, reached " zero scaling loss " that alloying element adds.
2) first vanadium metal (V) is used for the modification of lead-free brazing.
Vanadium metal (V) and two kinds of elements compounding of rare earth element nd are added; Through optimizing the chemical composition of V, Nd and Sn, Cu, Ni; Utilize V, " cooperative effect " of two kinds of trace elements of Nd in Sn-Cu-Ni; Improve wetting, the spreading property of solder significantly, greatly improved the tissue of solder, improved the mechanical property (σ of its solder joint (or brazed seam)
b, τ) performance of antifatigue especially, greatly optimized, improved the combination property of Sn-Cu-Ni solder.
Table 1: the Sn-Cu-Ni lead-free solder alloy composition (wt.%) that typically contains V, Nd and Ge
3) test is found; In the composition range of the selected Sn-Cu-Ni series leadless solder of the present invention, add rare earth element nd, because " surface-active " effect; Can significantly improve the brazing property of Sn-Cu-Ni brazing filler metal alloy; Simultaneously can deoxidation and desulfurization, stop the molten solder surface oxidation, suppressed Cu in the liquid molten solder simultaneously
6Sn
5Deng the formation of intermetallic compound with grow up, improved the flowability of liquid solder, it is better that it is sprawled with wettability.And the experimental study result finds element V and the compound interpolation of Nd; Have other rare earth (like La, Ce, Er, Y, Lu etc.) better optimize function of organization (referring to accompanying drawing 4,5,6), and be not only the effect of traditional in the past thinning microstructure than independent interpolation Nd and existing document or patent report; Produce synergy with V after adding rare earth element nd, improve the soldering Interface Microstructure, improve bond strength and anti-fatigue performance, guaranteed the reliability of soldered fitting under hot conditions.Test shows that the addition of rare earth element nd (mass percent) was less than 0.001% o'clock, and it is very little that the Sn-Cu-Ni solder performance is changed influence.After but addition surpasses 0.4%; Because oxidation is serious and Sn-Nd, the Sn-V-Nd compound of generation bulk; Obviously weaken the Sn-Cu-Ni series leadless solder wetability, brazed seam mechanical property and the optimization effect; Therefore, confirmed the upper and lower bound of Nd constituent content, content should be controlled at (in the scope of 0.001wt.%～0.4wt.%).
The large dendritic crystal that the compound interpolation of V and Nd obviously produces in the refinement brazing filler metal alloy process of setting obviously increases the ratio of fine and closely woven eutectic structure, makes soldered fitting have excellent mechanical property.Can find out (referring to accompanying drawing 4,5,6) from result of the test: the adding of V and Nd has obviously changed the pattern of solder microscopic structure, and the difference of Nd element addition has produced remarkable influence to eutectic structure.Generate stable, tiny, fine and close compound with constituent element; Separate out simultaneously at intracrystalline and crystal boundary; Suppressed dislocation motion, the second-phase dispersion degree of intracrystalline and crystal boundary is very high, significantly improves the grain coarsening temperature; The brazed seam tensile strength of solder and anti-fatigue performance also obviously improve, and have improved the reliability of soldered fitting.
4) adding of trace V and Nd element is also found in experimental study among the present invention, especially when the content of V and Nd is close, can significantly optimize second phase (the intermetallic compound Cu of Sn-Cu-Ni solder
6Sn
5, (Cu, Ni)
6Sn
5) institutional framework, reduce elemental diffusion speed, suppress excessively growing up of intermetallic compounds layer in the soldered fitting, make welding point have excellent mechanical property, improved the anti-fatigue performance of soldered fitting.
5) first metal Ge element is used for lead-free brazing, can not only improves the antioxygenic property in solder production and the use, also can improve the wettability of lead-free brazing.The addition of Ge is in 0.001wt.%～0.1wt.% scope; Ge is present in crystal boundary, has stoped growing up of crystal grain, and the while has also prevented the generation of oxide in the solder melt structure and grown up; To improving the non-oxidizability of solder, improve wettability and played great effect.
Compare with former studies, creativeness of the present invention is:
One, first with rare earth elemental metals neodymium (Nd) and the compound interpolation of metallic element vanadium (V), is aided with germanium metal (Ge) element, in order to the microscopic structure of refinement Sn-Cu-Ni lead-free brazing, improve its brazing property and improve the mechanical property of solder joint (brazed seam).The design of employing orthogonal optimization through a large amount of contrast tests, has confirmed to have the novel alloy system of excellent comprehensive performance: the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge.Through the optimizing components test, confirmed the content range of each constituent element respectively.
The compound interpolation of trace element V, Nd, Ge has produced tangible optimization effect to the performance of solder: under the reciprocation of three kinds of trace elements; The flowability of liquid solder has obtained enhancing; Significantly reduced solder oxidation in use; Obviously improved the form of solder joint, the various defectives of solder joint (brazed seam) obviously reduce.Especially in brazing process, V and Nd form tiny, fine and close, even, continuous compound layer with Sn at the interface solder and mother metal, separate out simultaneously at intracrystalline and crystal boundary, have suppressed the motion of dislocation at intracrystalline and crystal boundary, have improved resistance of deformation.Meanwhile; Optimized the orientation of intermetallic compounds layer at the interface; And has excellent lattice matching between mother metal and the solder matrix; Improve the bond strength and the anti-fatigue performance of soldered fitting, guaranteed the reliability (referring to Fig. 1 a, 1b, Fig. 3, Fig. 7 a and Fig. 7 b) during soldered fitting under arms.
Two, good wettability is the important prerequisite condition that can solder drop into practical application, also is the bottleneck that lead-free brazing runs in evolution.To the mensuration of Sn-Cu-Ni lead-free brazing wettability, sprawl the spreading property that experimental evidence standard GB/T 11364-2008 " solder wetting property test method " measures solder.A large amount of result of the tests show, the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is wetting, spreading property significantly is superior to existing Sn-Cu-Ni series leadless solder.The compound interpolation of V, Nd and Ge has reduced the surface tension coefficient of liquid solder effectively, promotes interfacial reaction to improve wettability simultaneously, and brazing property has obtained tangible optimization.Result of the test shows: the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge of the present invention cooperates commercially available no-clean scaling powder (RMA type), wetability, spreadability good (referring to Fig. 2) on red copper and pcb board.
Fig. 1 a and Fig. 1 b have all illustrated the heterogeneity brazing filler metal alloy promptly by the mechanical property of the solder of 1,2,3,4,5 and 6 six numbering shown in the aforesaid table 1; Wherein: Fig. 1 a has illustrated QFP device (the i.e. four limit flat package devices of different Nd content; Quad Flat Package is called for short QFP) solder joint (nonageing and 150 ℃ of timeliness 500h) tensile force; And Fig. 1 b has illustrated plate resistor (nonageing and 150 ℃ of timeliness 500h) the solder joint shearing resistance of different Nd content; Thereby the solder joint (brazed seam) that can find neoteric Sn-Cu-Ni-V-Nd-Ge lead-free brazing after postwelding and Ageing Treatment mechanical property (according to the general requirement regulation of electronic device; Tensile force and shearing resistance are the bigger the better) all be superior to not containing the common Sn-Cu-Ni solder of Nd, the optimum content of Nd is between 0.03wt.%～0.2wt.%.
What Fig. 2 illustrated is the heterogeneity brazing filler metal alloy spreading area by 1 shown in the table 1,2,3,4,5 and 6 these six numberings, six values of the mass percent of Nd: [contain X wt.%Nd (X=0.001,0.03; 0.05,0.1,0.2; 0.4)], 0.05wt.%V, 0.01wt.%Ge; 0.7wt.%Cu, 0.05wt.%Ni, surplus is Sn).
Wherein: sprawl spreading property that experimental basis standard GB/T 11364-2008 " solder wetting property test method " measures solder (according to the general requirement of soldering; Solder " spreading area " is big more; Explain that the solder spreading property is good more, explain that simultaneously solder is good more to the wettability of mother metal).
Fig. 3 is same test conditions following fatigue life of the cycle (be defined as load and descend 50%, test temperature is 25 ℃, total range of strain ε=0.006, test frequency is 0.5Hz) of heterogeneity brazing filler metal alloy in the table 1 (solder sequence number 1,2,3,4,5,6).According to the common technology assessment regulation of metal material, metal material is many more at same test conditions following fatigue life of cycle, shows the fatigue life good more (long more) of material.
Fig. 4 is the metallographic microstructure that do not add the Sn-Cu-Ni lead-free solder alloy of V, Ge and rare earth Nd (contains 0.7wt.%Cu, 0.05wt.%Ni, surplus is the solder microscopic structure (100 *) of Sn (not adding rare earth element)).
Fig. 5 is the metallographic microstructure (* 100) that adds the Sn-Cu-Ni lead-free solder alloy of V, Ge and rare earth Nd (0.05wt.%), and the directionality of comparing common Sn-Cu-Ni lead-free brazing dendrite obviously reduces, and " there is pattern in eutectic structure " obviously changes; Primary crystal β-Sn ratio obviously reduces in the tissue, and even tissue (contains 0.05wt.%V, 0.05wt.%Nd; 0.05wt.%Ge, 0.7wt.%Cu, 0.05wt.%Ni;, surplus is the solder microscopic structure (100 *) of Sn).
Fig. 6 is the metallographic microstructure (* 100) that adds the Sn-Cu-Ni lead-free solder alloy of V, Ge and 0.4wt.% rare earth Nd; The pattern of intermetallic compound, size and distribution (contain 0.05wt.%V in the solder matrix; 0.4wt.%Nd, 0.05wt.%Ge, 0.7wt.%Cu; 0.05wt.%Ni, surplus is the solder microscopic structure (100 *) of Sn).
Fig. 7 a and Fig. 7 b are welding point interface microscopic structure (150 ℃ of timeliness 500h).Wherein: Fig. 7 a for do not add V, Ge and rare earth Nd the unleaded welding point interface microscopic structure of Sn-Cu-Ni (contain 0.7wt.%Cu, 0.05wt.%Ni, surplus is the Sn welding point interface microscopic structure of (not adding V, Nd, Ge element) (150 ℃ of timeliness 500h); Fig. 7 b (contains 0.05wt.%V for the unleaded welding point interface microscopic structure of Sn-Cu-Ni of adding 0.4wt.% rare earth Nd, V and Ge; 0.4wt.%Nd; 0.1wt.%Ge; 0.7wt.%Cu, 0.05wt.%Ni, surplus is the welding point interface microscopic structure (150 ℃ of timeliness 500h) of Sn; Interfacial brittle intermetallic compounds layer thickness is compared the unleaded solder joint of common Sn-Cu-Ni and is obviously reduced, and explains that neoteric lead-free solder alloy system compares common Sn-Cu-Ni solder joint that lead-free brazing constitutes fatigue behaviour in its military service process and be significantly improved.
Embodiment:
According to the quality proportioning of " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " of the present invention, the narration embodiments of the invention.
Embodiment one
A kind of Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is pressed the mass percent proportioning, and its composition is: 0.07%Cu, and 0.8%Ni, 0.001%V, 0.1%Nd, 0.005%Ge, surplus is Sn.Solidus temperature is about 220 ℃ for " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " that the mentioned component proportioning obtains, and liquidus temperature (has been considered test error) about 227 ℃.Spreading area on copper plate is 62mm
2, the tensile force 11.3N of QFP solder joint, plate resistor shearing strength (power) is 71N, cycle fatigue life of solder joint is 92 * 10
3
Embodiment two
A kind of Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is pressed the mass percent proportioning, and its composition is: 1.8%Cu, and 0.4%Ni, 0.1%V, 0.03%Nd, 0.1%Ge, surplus is Sn.Solidus temperature is about 217 ℃ for " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " that the mentioned component proportioning obtains, and liquidus temperature (has been considered test error) about 225 ℃.Spreading area on copper plate is 54mm
2, the tensile force 10.8N of QFP solder joint, plate resistor shearing strength (power) is 65N, cycle fatigue life of solder joint is 86 * 10
3
Embodiment three
A kind of Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is pressed the mass percent proportioning, and its composition is: 0.2%Cu, and 2.0%Ni, 0.005%V, 0.001%Nd, 0.06%Ge, surplus is Sn.Solidus temperature is about 219 ℃ for " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " that the mentioned component proportioning obtains, and liquidus temperature (has been considered test error) about 226 ℃.Spreading area on copper plate is 46mm
2, the tensile force 10.1N of QFP solder joint, plate resistor shearing strength (power) is 60N, cycle fatigue life of solder joint is 55 * 10
3
Embodiment four
A kind of Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is pressed the mass percent proportioning, and its composition is: 0.7%Cu, and 0.01%Ni, 0.1%V, 0.4%Nd, 0.05%Ge, surplus is Sn.Solidus temperature is about 219 ℃ for " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " that the mentioned component proportioning obtains, and liquidus temperature (has been considered test error) about 225 ℃.Spreading area on copper plate is 48mm
2, the tensile force 10.5N of QFP solder joint, plate resistor shearing strength (power) is 67N, cycle fatigue life of solder joint is 60 * 10
3
Embodiment five
A kind of Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is pressed the mass percent proportioning, and its composition is: 0.7%Cu, and 0.05%Ni, 0.4%V, 0.05%Nd, 0.001%Ge, surplus is Sn.Solidus temperature is about 219 ℃ for " the Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge " that the mentioned component proportioning obtains, and liquidus temperature (has been considered test error) about 223 ℃.Spreading area on copper plate is 65mm
2, the tensile force 11.9N of QFP solder joint, plate resistor shearing strength (power) is 74N, cycle fatigue life of solder joint is 102 * 10
3
For the ease of contrast, the present invention has chosen the Sn-Cu-Ni solder that does not add V, Nd and Ge and has carried out the test of correlated performance index.Its composition (mass percent) is: 1.5% Cu, and 1.3% Ni, 0.05%Pb, surplus is Sn.Test determination goes out its solidus temperature about 224 ℃, and liquidus temperature (has been considered test error) about 227 ℃; Spreading area on copper plate is 44mm
2, the tensile force 8.6N of QFP solder joint, plate resistor shearing strength (power) is 47N, cycle fatigue life of solder joint is 50 * 10
3
Can find that from embodiment contain the Sn-Cu-Ni solder of Pr, Sr and Ga, its solidus temperature is about 217 ℃, liquidus temperature (has been considered test error) about 227 ℃.Spreading area on copper plate is at 46mm
2～65mm
2Scope is (all greater than 44mm
2), the tensile force of QFP solder joint is at 10.1N～11.9N scope (all greater than 8.6N), the plate resistor shearing strength is at 60N～74N scope (all greater than 47N), solder joint fatigue life cycle 55 * 10
3～102 * 10
3Scope is (all greater than 50 * 10
3).
Claims (1)
1. a Sn-Cu-Ni lead-free brazing that contains V, Nd and Ge is characterized in that its chemical composition by the mass percent proportioning is: 0.07～1.8% Cu, 0.01～2.0% Ni; 0.001～0.1% V; 0.001～0.4% Nd, 0.001～0.1% Ge, surplus is Sn.
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| CN102794578B (en) * | 2012-08-10 | 2015-04-22 | 大连理工大学 | Brazing filler metal for brazing titanium alloy and steel or titanium aluminum alloy as well as steel |
| CN102974954B (en) * | 2012-12-17 | 2015-03-11 | 南京航空航天大学 | Tin-copper-nickel (Sn-Cu-Ni) lead-free solder containing ferrum (Fe) and praseodymium (Pr) |
| CN104668792B (en) * | 2013-11-28 | 2017-01-11 | 中国科学院金属研究所 | Controllable preparation method of tin and indium interconnection welding spot IMCs ( intermetallic compounds) |
| CN109277721B (en) * | 2018-09-20 | 2020-11-27 | 常熟市华银焊料有限公司 | Sn-Cu-Ni lead-free solder containing Ga and Nd |
| CN109048114B (en) * | 2018-09-20 | 2021-02-12 | 南京理工大学 | Sn-Cu-Ni lead-free solder containing Ga and Nd |
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| CN101885119A (en) | 2010-11-17 |
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