CN101219507A - Leadless welding material and method for producing the same - Google Patents
Leadless welding material and method for producing the same Download PDFInfo
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- CN101219507A CN101219507A CNA2008100705774A CN200810070577A CN101219507A CN 101219507 A CN101219507 A CN 101219507A CN A2008100705774 A CNA2008100705774 A CN A2008100705774A CN 200810070577 A CN200810070577 A CN 200810070577A CN 101219507 A CN101219507 A CN 101219507A
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Abstract
A lead-free solder and a preparation method thereof are provided, which relate to a metal alloy, in particular to a novel low cost high temperature lead-free solder alloy applied to graded packaging and a preparation method thereof. The invention provides a lead-free solder which has melting temperature up to 300 DEG C, excellent wetting property and electrical properties, low raw material cost, simple preparation process, short period and can replace the traditional solder alloy of Sn-95wt percent Pb and a preparation method thereof. The components of the solder comprise antimony of 28-32 wt percent, copper of 10-15 wt percent, silver of 7-10 wt percent, yttrium of 0.2-0.5 wt percent and stannum of the rest wt percent. The raw materials of antimony, copper, silver, yttrium and stannum are vacuum packaged with vacuum degree less than 5Pa and then argon gas is filled in. the packaged raw materials are put into a reacting furnace to be melted and heat treated with heat treatment temperature between 600-950 DEG C, heat preserved for at least 24h, icy water quenched, vacuum packaged and annealed at temperature between 150-250 DEG C, finally the invention is obtained.
Description
Technical field
The present invention relates to a kind of metal alloy, especially relate to a kind of novel low-cost high-temperature leadless welding material Alloy And Preparation Method of classification encapsulation usefulness.
Background technology
Along with environment pollution and health problem has become the focus that the whole world is paid close attention to, the Electronic Packaging industry faces is to the challenge of " green " unleaded transformation, European Union has issued " waste electrical and electronic equipment (WEEE) " and " banning use of some harmful substance (RHOS) about electronic electric equipment " two decrees, from on July 1st, 2006, completely forbid leaded electronic product import, adopting the Lead-free in Electronic Packaging material is the trend of the times of welding material and technological development in the Electronic Packaging industry.
Now, in semiconductor classification packaging technology, at present the high temperature solder materials that uses but still be traditional leaded Sn-95wt%Pb welding material (fusing point is 300 ℃) and unleaded Sn-80wt%Au welding material (280 ℃ of fusing points) (1, Liu Zeguang, Guo Gensheng, Luo Ximing, Deng. the performance of golden tin composite soldering and application [J]. noble metal, 1997 (suppl): 425; 2, Liu Zeguang, Yang Futao, Gu Kaiyuan. the manufacture method of aurum tin soldering material [P]. China. invention .CN 1026394C, 11.25.1999).Yet for to environmental protection and consider expensive reason, the application of this two classes scolder also is very limited.How to improve the service temperature scope that existing lead-free solder can bear, perhaps developing new solder compositions, to adapt to high-temperature applications be extremely important and a be not well studied problem.Development along with electronic devices and components high speed, multifunction, in many electronics industries of modern times in the welding of the complicated components and parts of multilayer, when encapsulating as multicore tablet mode MCM (Multi-Chip Module), usually adopt substep welding (Step Soldering) to need the scolder of a series of different melting points scopes, (3, (day) villous themeda natural pond gram is clear. pb-free solder technology [M]. Beijing: Science Press, 2004; 4, Guo Fu. unleaded soldering tech and application [M]. Beijing: Science Press, 2006.) this neither be traditional the Sn-Pb alloy can satisfy.
Therefore, the high-temp leadless welding material for development of new just seems more important.At present, the lead-free solder of studying concentrates on middle low temperature range mostly, especially with SnAgCu ternary system and SnAg binary system in the majority (5, Shi Yaowu, thunder Yongping .SnAgCu series leadless solder technical developments [J] such as Xia Zhidong. industry forward position, 2004,4:10-16), yet their fusing point concentrates near 218 ℃ mostly, and near also only 250 ℃ (the SnSb binary system alloy) of high-temperature scope can not satisfy the condition that encapsulates under high temperature (300 ℃) slightly.Scarcely belong to Sn base alloy at some high temperature alloys that grind in addition, but belong to AuSi series alloy (6, Mo Wenjian, Wang Zhifa, Jiang Guosheng, the research of warm eutectic solder during .Au-Ag-Si such as Wang Haishan are novel. Rare Metals Materials and engineering, 2005,134 (3)), cost is higher, is subjected to very big restriction in the application.
Summary of the invention
The object of the present invention is to provide a kind of fusion temperature can reach 300 ℃, comparatively good on wetability and electric property, cost of material is low, and preparation technology is simple, cycle is short, can replace leadless welding material of traditional Sn-95wt%Pb solder alloy (fusing point is 300 ℃) and preparation method thereof.
The composition of leadless welding material of the present invention and by mass percentage content be: antimony 28%～32%, copper 10%～15%, silver 7%～10%, yttrium 0.2%～0.5%, Yu Weixi.
The preparation method of leadless welding material of the present invention may further comprise the steps:
1) with antimony, copper, silver, yttrium and tin raw material Vacuum Package, vacuum charges into argon gas then below 5Pa;
2) above-mentioned packaged antimony, copper, silver, yttrium and tin raw material being put into the reacting furnace smelting heat handles, heat treatment temperature is 600～950 ℃, and temperature retention time is at least more than the 24h, ice water quenching, anneal down at 150～250 ℃ after the Vacuum Package again, promptly obtain the SnSbCuAgY leadless welding material.
Charge into argon gas to (0.7～0.8) * 10
5Pa.Heat treatment temperature is preferably 850～900 ℃, and 24h at least anneals.
To after taking out, the alloy after the Overheating Treatment carry out Vacuum Package, best homogenizing annealing afterwards, and purpose is in order to guarantee that DSC tests the stability of equilibrium of required sample and eliminates internal stress, but annealing temperature can not be higher than 250 ℃, prevents solder fusing.
For sample is carried out the test of electric property and wetability, the SnSbCuAgY leadless welding material sample that obtains can be cut into required shape with the method that line cuts.The thickness of sheet leadless welding material sample is about 0.4～0.8mm, and the diameter of disc shaped test piece is not less than 1mm, but also unsuitable excessive, to guarantee experimental precision.
The prepared SnSbCuAgY high temperature lead-free solder of the present invention alloy has the following advantages: on the basis of SnSb bianry alloy, adopt multi-element alloyed method, by add properly mixed Cu, Ag, Y element makes it form stable middle phase in alloying process, thereby the fusing point of this leadless welding alloy is improved, reaches 300 ℃.Cut into slices by the method for line cutting through the alloy that this method obtains; and carry out the test of wetability experiment and electric conductivity; experimental result shows; this solder alloy has under protective atmosphere and Cu substrate wetting power preferably; and its electric conductivity is similar with the most ripe up to now SnAgCu lead-free solder; the angle of wetting of this alloy and Cu substrate reaches 33～35 degree, and resistivity is (0.37～0.43) * 10
-6Ω m.
SnSbCuAgY high-temp leadless welding material of the present invention can be used as special scolder at high temperature (＞300 ℃) carry out classification encapsulation, such as engineering fields such as nuclear power, Aero-Space, automobile, chemical industry potential application prospect is being arranged, and preparation technology is simple, and the cycle is short, and is with low cost.
Description of drawings
Fig. 1 calculates phasor for the Sn-Sb-Cu-Ag vertical section.In Fig. 1, abscissa be silver mass percent Wt (%) Ag, ordinate be temperature T emperature (℃).The zone that is identified among the figure is respectively liquid phase region Liquid, solid-liquid two-phase region Cu
3Sn+CuInSn_E+Liquid+SbSn, solid phase area CuInSn_E+Hcp_A
3+ SbSn.
Fig. 2 is that the Sn30Sb13Cu7.5Ag0.2Y solder alloy is at 900 ℃ of insulation 24～36h, the DSC curve after the ice water quenching.In Fig. 2, abscissa be temperature T emperature (℃), ordinate is heat flow Heating flow (mw/mg), the fusion temperature scope is 301～333 ℃.
Fig. 3 is that the Sn30Sb13Cu8.0Ag0.3Y solder alloy is at 900 ℃ of insulation 24～36h, the DSC curve after the ice water quenching.In Fig. 3, abscissa be temperature T emperature (℃), ordinate is heat flow Heating flow (mw/mg), the fusion temperature scope is 302～335 ℃.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1: preparation Sn30Sb13Cu7.5Ag0.2Y solder alloy
Take by weighing 30% purity and be 99.9% antimony, 13% purity and be 99.5% copper, 7.5% purity and be 99.9% silver, 0.2% purity and be 99.99% yttrium and surplus purity and be 99.5% tin.Material vacuums such as above-mentioned antimony, copper, silver, yttrium, tin are encapsulated in the quartz ampoule, guarantee that vacuum reaches below the 5Pa in the quartz ampoule, charge into high-purity argon gas then to (0.7～0.8) * 10
5Pa handles 850 ℃ of reacting furnace smelting heat afterwards, and temperature retention time reaches 24～36h, promptly obtains SnSbCuAgY high-temp leadless welding material alloy.To carry out ice water quenching rapidly after the taking-up of the heat treated SnSbCuAgY high-temp leadless of above-mentioned process welding material alloy, again it is carried out afterwards putting into 200 ℃ of baking oven homogenizing annealings 24h at least after the quartz ampoule Vacuum Package, take out the method for utilizing the line cutting after the cooling cut into slices (thickness 0.4～0.8mm) and discoid material, promptly finally obtain the DSC sample of requirement of the present invention and the specimen size of test electric property and wetability, the calculating phasor of this solder alloy as shown in Figure 1.
Adopt German Netzsch STA 404 to carry out the DSC test, heating rate is 2 ℃/min, sample quality is less than 20mg, resulting DSC curve as shown in Figure 2, the fusion temperature scope that can obtain this solder alloy from Fig. 2 is 301～333 ℃, wherein, solidus temperature is 301 ℃, and liquidus temperature is 333 ℃.Solder alloy composition and fusion temperature see Table 1.
Table 1 solder alloy composition and fusion temperature
| Specimen coding | Alloying component (wt%) | Fusion range (℃) | |||||
| Sn | Sb | Cu | Ag | Y | Solidus | Liquidus curve | |
| 1 | 49.3 | 30 | 13 | 7.5 | 0.2 | 301 | 333 |
| 2 | 49.7 | 28 | 15 | 7 | 0.3 | 302 | 335 |
| 3 | 48.6 | 32 | 10 | 9 | 0.4 | 300 | 332 |
| 4 | 46.5 | 31 | 14 | 8 | 0.5 | 298 | 336 |
Adopt OTF-1200X vacuum heat treatment furnace and German Kruss DSA 100 to carry out the wettability test of above-mentioned alloy; obtain under protective atmosphere (mixture of hydrogen and nitrogen) condition; the angle of wetting of this scolder and Cu substrate (industrial copper sheet T3) reaches 35 degree, and is as shown in table 2.
The wetability of table 2 solder alloy
| Sample | Reaction atmosphere | Angle of wetting (°) |
| Sn30Sb13Cu7.5Ag0.2Y | Protective atmosphere (mixture of hydrogen and nitrogen) | 35 |
| Sn28Sb15Cu7.0Ag0.3Y | Protective atmosphere (mixture of hydrogen and nitrogen) | 33 |
| Sn32Sb10Cu9.0Ag0.4Y | Protective atmosphere (mixture of hydrogen and nitrogen) | 36 |
| Sn29Sb12Cu10Ag0.3Y | Protective atmosphere (mixture of hydrogen and nitrogen) | 33 |
Adopt the digital four point probe tester of SX1934 type to carry out the resistivity measurement of above-mentioned alloy, the resistivity that obtains this scolder is 0.374 * 10
-6Ω m, as shown in table 3.
Table 3: the wetability of solder alloy
| Sample | Reaction atmosphere | Angle of wetting (°) |
| Sn30Sb13Cu7.5Ag0.2Y | In the air | 68 |
| Protective atmosphere (H 2+N 2) | 35 | |
| Sn28Sb15Cu7.0Ag0.3Y | In the air | 65 |
| Protective atmosphere (H 2+N 2) | 33 | |
| Sn32Sb10Cu9.0Ag0.4Y | In the air | 70 |
| Protective atmosphere (H 2+N 2) | 36 |
Embodiment 2: preparation Sn28Sb15Cu7Ag0.3Y solder alloy
Take by weighing 28% purity and be 99.9% antimony, 15% purity and be 99.5% copper, 7% purity and be 99.9% silver, 0.3% purity and be 99.99% yttrium and surplus purity and be 99.5% tin.Material vacuums such as above-mentioned antimony, copper, silver, yttrium, tin are encapsulated in the quartz ampoule, guarantee that vacuum reaches below the 5Pa in the quartz ampoule, charge into high-purity argon gas then to (0.7～0.8) * 10
5Pa handles 900 ℃ of reacting furnace smelting heat afterwards, and temperature retention time reaches 24～36h, promptly obtains SnSbCuAgY high-temp leadless welding material alloy.To carry out ice water quenching rapidly after the taking-up of the heat treated SnSbCuAgY high-temp leadless of above-mentioned process welding material alloy, again it is carried out afterwards putting into 200 ℃ of baking oven homogenizing annealings 24h at least after the quartz ampoule Vacuum Package, take out the method for utilizing the line cutting after the cooling cut into slices (thickness 0.4～0.8mm) and discoid material, promptly finally obtain the DSC sample of requirement of the present invention and the specimen size of test electric property and wetability, the calculating phasor of this solder alloy as shown in Figure 1.
Adopt German Netzsch STA 404 to carry out the DSC test, heating rate is 2 ℃/min, sample quality is less than 20mg, resulting DSC curve as shown in Figure 3, the fusion temperature scope that can obtain this solder alloy from Fig. 3 is 302～335 ℃, wherein, solidus temperature is 302 ℃, and liquidus temperature is 335 ℃.
Adopt OTF-1200X vacuum heat treatment furnace and German Kruss DSA 100 to carry out the wettability test of above-mentioned alloy; obtain under protective atmosphere (mixture of hydrogen and nitrogen) condition; the angle of wetting of this scolder and Cu substrate (industrial copper sheet T3) reaches 33 degree, and is as shown in table 2.
Adopt the digital four point probe tester of SX1934 type to carry out the resistivity measurement of above-mentioned alloy, the resistivity that obtains this scolder is 0.398 * 10
-6Ω m, as shown in table 4.
The resistivity of table 4 solder alloy
| Sample | Electricalresistivity's reading (m Ω cm) | Thickness (mm) | Correction factor G | The electricalresistivity On average (μΩm) |
| Sn30Sb13Cu7.5Ag0.2Y | 0.096 | 0.54 | 0.389 | 0.374 |
| Sn28Sb15Cu7.0Ag0.3Y | 0.099 | 0.56 | 0.402 | 0.398 |
| Sn32Sb10Cu9.0Ag0.4Y | 1.158 | 0.51 | 0.368 | 0.426 |
| Sn3.5Ag0.5Cu | - | - | - | 0.664 |
| Sn80Au | - | - | - | 0.164 |
Annotate: Sn3Ag0.5Cu, Sn80Au scolder data from document, correction factor G derives from the digital four point probe tester of SX1934 appendix.(7, Xue Songbai, Liu Lin, Dai Yongfeng, Yao Lihua etc. the trace rare-earth element cerium is to Sn-Ag-Cu lead-free brazing physical property and solder joint effects of tensile strength. the welding journal 2005,126 (10)).
Above result shows, under the prerequisite of rational proportion, constituent content is wherein finely tuned, trace as yttrium increases progressively, angle of wetting will be had slightly to be reduced, this mainly is because the adding of rare earth element yttrium causes the growth of its diffusion layer, impels the surface to increase, thereby has promoted the raising of wetting power.
Embodiment 3: preparation Sn32Sb10Cu9Ag0.4Y solder alloy
Take by weighing 32% purity and be 99.9% antimony, 10% purity and be 99.5% copper, 9% purity and be 99.9% silver, 0.4% purity and be 99.99% yttrium and surplus purity and be 99.5% tin.Method according to embodiment 1 prepares this solder, and wherein, heat treatment temperature is 750 ℃.
Adopt German Netzsch STA 404 to carry out the DSC test, heating rate is 2 ℃/min, and sample quality is less than 20mg, and the fusion temperature scope that records this solder alloy is 300～332 ℃.
Adopt OTF-1200X vacuum heat treatment furnace and German Kruss DSA 100 to carry out the wettability test of above-mentioned alloy; obtain under protective atmosphere (mixture of hydrogen and nitrogen) condition; the angle of wetting of this scolder and Cu substrate (industrial copper sheet T3) reaches 36 degree, and is as shown in table 2.
Adopt the digital four point probe tester of SX1934 type to carry out the resistivity measurement of above-mentioned alloy, the resistivity that obtains this scolder is 0.426 * 10
-6Ω m, as shown in table 4.
Embodiment 4: preparation Sn31Sb14Cu8Ag0.5Y solder alloy
Take by weighing 31% purity and be 99.9% antimony, 14% purity and be 99.5% copper, 8% purity and be 99.9% silver, 0.5% purity and be 99.99% yttrium and surplus purity and be 99.5% tin.The preparation method is identical with embodiment 1, and heat treatment temperature is 800 ℃.
Embodiment 5 and 6: preparation Sn29Sb12Cu10Ag0.3Y and Sn30Sb11Cu8.5Ag0.2Y solder alloy
Take by weighing 29%, 30% purity respectively and be 99.9% antimony, 12%, 11% purity and be 99.5% copper, 10%, 8.5% purity and be 99.9% silver, 0.3%, 0.2% purity and be 99.99% yttrium and surplus purity and be 99.5% tin.Method according to embodiment 1 prepares this solder, and wherein, heat treatment temperature is respectively 600 ℃ and 900 ℃.
Adopt German Kruss DSA 100 to carry out the wettability test of above-mentioned alloy, obtain under the air atmosphere condition, the angle of wetting of this scolder and Cu substrate (industrial copper sheet T3) is 65～68 ℃, and is as shown in table 3.
When above presentation of results, scolder reacted with the Cu substrate in air, oxidation had taken place in the Cu substrate, causes its wetability sharply to descend.
Claims (5)
1. leadless welding material, it is characterized in that its composition and by mass percentage content be: antimony 28%～32%, copper 10%～15%, silver 7%～10%, yttrium 0.2%～0.5%, Yu Weixi.
2. the preparation method of leadless welding material as claimed in claim 1 is characterized in that may further comprise the steps:
1) with antimony, copper, silver, yttrium and tin raw material Vacuum Package, vacuum charges into argon gas then below 5Pa;
2) above-mentioned packaged antimony, copper, silver, yttrium and tin raw material being put into the reacting furnace smelting heat handles, heat treatment temperature is 600～950 ℃, and temperature retention time is at least more than the 24h, ice water quenching, anneal down at 150～250 ℃ after the Vacuum Package again, promptly obtain the SnSbCuAgY leadless welding material.
3. the preparation method of leadless welding material as claimed in claim 2 is characterized in that charging into argon gas to (0.7～0.8) * 10
5Pa.
4. the preparation method of leadless welding material as claimed in claim 2 is characterized in that heat treatment temperature is 850～900 ℃.
5. the preparation method of leadless welding material as claimed in claim 2,24h at least is characterized in that annealing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864511B (en) * | 2009-04-20 | 2012-06-27 | 无锡日月合金材料有限公司 | Annealing process of sealing welding flux |
| CN106825979A (en) * | 2017-01-04 | 2017-06-13 | 南京信息工程大学 | A kind of low melting point Sn Zn Bi Mg series lead-free solders and preparation method thereof |
| CN107498211A (en) * | 2017-10-18 | 2017-12-22 | 镇江市锶达合金材料有限公司 | A kind of pb-free solder material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11291083A (en) * | 1998-04-14 | 1999-10-26 | Murata Mfg Co Ltd | Solder alloy |
| JP4609296B2 (en) * | 2005-12-05 | 2011-01-12 | 株式会社日立製作所 | High temperature solder, high temperature solder paste material, and power semiconductor device using the same |
-
2008
- 2008-01-29 CN CN2008100705774A patent/CN101219507B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864511B (en) * | 2009-04-20 | 2012-06-27 | 无锡日月合金材料有限公司 | Annealing process of sealing welding flux |
| CN106825979A (en) * | 2017-01-04 | 2017-06-13 | 南京信息工程大学 | A kind of low melting point Sn Zn Bi Mg series lead-free solders and preparation method thereof |
| CN106825979B (en) * | 2017-01-04 | 2019-11-12 | 南京信息工程大学 | A kind of low melting point Sn-Zn-Bi-Mg series lead-free solder and preparation method thereof |
| CN107498211A (en) * | 2017-10-18 | 2017-12-22 | 镇江市锶达合金材料有限公司 | A kind of pb-free solder material and preparation method thereof |
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