CN101992362A - Oxidation-resistant lead-free solder alloy suitable for powder process - Google Patents
Oxidation-resistant lead-free solder alloy suitable for powder process Download PDFInfo
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- CN101992362A CN101992362A CN 201010571011 CN201010571011A CN101992362A CN 101992362 A CN101992362 A CN 101992362A CN 201010571011 CN201010571011 CN 201010571011 CN 201010571011 A CN201010571011 A CN 201010571011A CN 101992362 A CN101992362 A CN 101992362A
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Abstract
The invention relates to an oxidation-resistant lead-free solder alloy suitable for a powder process, in particular to a lead-free solder composition, more particular to a lead-free solder composition which is suitable for a powder process and has lower silver content. The alloy comprises the following components in percent by weight: 0.05-1.0 percent of Ag, 0.05-1.0 percent of Cu, 0.05-0.5 percent of Sb, 0.005-0.1 percent of Ge and the balance of Sn. The lead-free low-silver solder suitable for the powder process has an oxidation resistance capability and can meet the requirements for lead free and no halogenation of solder.
Description
Technical field:
The present invention relates to a kind of leadless welding alloy; Be particularly related to a kind of leadless welding alloy that can be made into alloy powder with oxidation resistance.
Background technology:
Developing rapidly of electronics and information industry causes the kind of electronic product sharply to increase, used scolder kind is assembled and encapsulated to electronic product also constantly to be increased, but after all, all be with tin as underlying metal, add different metals or nonmetalloid and constitute new solder compositions.Tin-lead solder still is extensive use of with characteristics such as its excellent wetability and weldability, electric conductivity, mechanical property, low costs; Along with the raising to further sound and people's environmental consciousness of protecting human laws and regulations, lead-free solder certainly will replace tin-lead solder.Present lead-free solder majority is that Xi-Yin, tin-copper, Sn-Bi, tin-silver-copper, Xi-Yin-bismuth, tin-copper-nickel, tin-zinc-copper etc. are formed or formed with above-mentioned alloy do basis interpolation trace element.To Xi-Yin, tin-copper, tin-copper-nickel system alloy, its wetability is relatively poor, and alloy structure is thick, and skewness is not suitable for making alloy powder; Sn-Bi, Xi-Yin-bismuth, tin-zinc-copper system are because its specific low melting point and electrode potential distribute only more suitable specific welding occasions.In the present lead-free solder, tin-silver-copper is that alloy has application promise in clinical practice, has obtained the recommendation of U.S. NEMI (National Electronics Manufacturing Initiative), Britain DTI (Department of Trade and Industry), STC (The Solder Technology Center) etc.Based on tin-silver-copper system, the most frequently used alloy is Sn-3Ag-0.5Cu (SAC305) and Sn-0.3Ag-0.7Cu (SAC0307), and its combination property is more superior.For SAC305, fatal weakness is because the use of a large amount of Ag causes its cost higher, and to SAC0307, its alloy structure is thick, and making the oxidation of alloy welding powder rear surface increases, be post processing, the realization of particularly not having halogen technology has brought bigger trouble.
Anti-oxidant for lead-free solder, industry way commonly used is independent or compound interpolation phosphorus (P), gallium (Ga) element in solder alloy at present, can both reach antioxidant effect preferably.But the solder alloy that adds P is not suitable for powder process, and the corrosion of die head because the adding of P easily causes dusting, and phosphide can not evenly cover the metal dust surface makes the powder can be anti-oxidant; Gallium compound is to being to play good antioxidant effect, but more difficult rupture of membranes during welding needs stronger scaling powder just can reach same welding effect, and this just causes final welded surface insulation resistance to descend.
Summary of the invention:
The leadless welding alloy with oxidation resistance that the purpose of this invention is to provide a kind of suitable powder process, it is a kind of have oxidation resistance, suitable unleaded low easy-flo of making alloy powder.
Technical solution of the present invention: solder alloy of the present invention, composed of the following components by weight percentage: Ag (silver) 0.05-1.0%, Cu (copper) 0.05-1.0%, Sb (antimony) 0.05-0.5%, Ge (germanium) 0.005-0.1%, surplus is Sn.
More than Ag content of the present invention be 0.25-0.80%.
Ag content of the present invention is 0.75%.
More than Cu content of the present invention be 0.05-0.80%.
Cu content of the present invention is 0.05%.
More than Sb content of the present invention be 0.16-0.38%.
Sb content of the present invention is 0.27%.
Ge content of the present invention is 0.021-0.074%.
More than Ge content of the present invention be 0.047%.
Can see from the phasor of Sn-Ag bianry alloy, the Sn-Ag formation solid solution that dissolves each other fully, and, improve mechanical property, especially the creep resistant fatigue behaviour of scolder because the adding of Ag can form Sn-Ag eutectic (Sn96.2Ag3.8) to reduce the fusing point of scolder.But after the addition of Ag surpassed 3.8%, along with the increase of Ag, the liquidus temperature of solder alloy sharply raise, and caused the rising of welding temperature and made electronic devices and components be subjected to fire damage; Secondly, Ag content increases the cost that has also directly increased solder alloy.Experimental results show that Ag content is 0.05-1.0%, be preferably 0.25-0.80%, further is 0.75%.
Interpolation Cu can make and form ternary eutectic between Sn-Ag-Cu to reduce the fusing point of scolder.The existence of Cu element both can improve the intensity of scolder, can strengthen the wetability of scolder again; The tensile strength of scolder also can obviously be strengthened because of the interpolation of Cu, and the affiliation that adds of Cu reduces the percentage elongation of scolder and the contraction percentage of area.Cu content is low excessively, and performance improvement is not obvious, the Cu too high levels, and the solder wettability variation forms the Sn-Cu intermetallic compound of fragility simultaneously, has reduced the bond strength of solder joint.Experiment showed, that Cu content is 0.05-1.0%, be preferably 0.05-0.80%, further is 0.05%.
Because the surface tension of Sb when liquid state only is 383 * 10
-5N/cm is far below 930 * 10 of Ag
-51300 * 10 of N/cm and Cu
-5N/cm also is lower than 566 * 10 of main metal Sn
-5N/cm, its adding can improve the wettability of solder alloy; But the addition with Sb increases, and alloy melting point can significantly rise, simultaneously, and the alloy phase change complexity.Experiment showed, that Sb content is 0.05-0.5%, be preferably 0.16-0.38%, further is 0.27%.
Oxidation resistance at alloy, adding rare earth element and inorganic elements P is one of effective way, but because its strong excessively catharsis and kelvin effect, form the collection skin layer of one deck structure exquisiteness, densification in the alloy atomization pulverizing process on the surface of metal powder grain, for further deep processing brings difficulty.And the Ge in the tetrels (germanium) has catharsis and kelvin effect to alloy equally, Ge has certain suction-operated to dissolved oxygen, the adding of Ge can make scolder be difficult for further oxidation, can crystal grain thinning after the adding, improve the apparent institutional framework of scolder drop in process of setting, the microstructure of scolder is played rotten stepless action.Addition as Ge is few, and performance is not had improvement substantially, too much can cause the melting solder surface viscosity to increase, and the alloyed powder sphericity of making is relatively poor, and the satellite ball increases.Experimental results show that Ge content is 0.005-0.1%, be preferably 0.021-0.074%, further is 0.047%.
The preparation method:
Low-silver lead-free solder of the present invention can be smelted by traditional approach, and promptly Sn, Ag, Cu, Sb are with the raw metal supply, and Ge adds with the form of intermediate alloy; Also can all adopt the form of intermediate alloy to add various alloying elements; Alloy preparation method is as follows:
Sn-Cu intermediate alloy: 99.95% smart Sn is joined in the graphite crucible, be warming up to 500-600 ℃ after the fusing, add 99.95% pure Cu.Smart Sn prepares by 90: 10 with the mass percent of pure Cu, stirs, and is incubated 60-120 minute, stirs, and it is 10% Sn-Cu intermediate alloy ingot that tapping casting one-tenth contains that Cu measures.
Sn-Ag intermediate alloy: 99.95% smart Sn is joined in the graphite crucible, be warming up to 500-600 ℃ after the fusing, add 99.95% pure Ag.Smart Sn prepares by 95: 5 with the mass percent of pure Ag, stirs, and is incubated 60-120 minute, stirs, and it is 5% Sn-Ag intermediate alloy ingot that tapping casting one-tenth contains that Ag measures.
Sn-Sb intermediate alloy: 99.95% smart Sn is joined in the graphite crucible, be warming up to 500-600 ℃ after the fusing, add 99.95% pure Sb.Smart Sn prepares by 95: 5 with the mass percent of pure Sb, stirs, and is incubated 60-120 minute, stirs, and it is 5% Sn-Sb intermediate alloy ingot that tapping casting one-tenth contains that Sb measures.
The Sn-Ge intermediate alloy: smart Sn with 99.95% and 99.95% Ge joined in the graphite crucible by weight 98: 2 and place vacuum melting furnace to carry out melting, be warming up to the fusion temperature of Ge, be incubated 60-120 minute, stirred 30 minutes, it is 2% Sn-Ge intermediate alloy ingot that tapping casting becomes to contain the Ge amount.
Calculate the good Sn-Cu intermediate alloy ingot of weighing, Sn-Ag intermediate alloy ingot, Sn-Sb intermediate alloy ingot, Sn-Ge intermediate alloy ingot, pure tin ingot by alloying component, the alloying component for preparing is adopted the crucible induction melting.Be stirred well to fusing fully, leave standstill a period of time, casting, the solder alloy ingot that obtains is by product such as the forms such as scolding tin rod, solder stick, solder ball (powder) and solder(ing) paste of further being processed into alloying component of the present invention.
Advantage:
(1) the effective refinement of adding of anti-oxidant element Ge the crystal grain of SAC alloy, and at the certain anti-oxidant collection skin layer of alloy powder surface formation, prevented the further oxidation of alloy fine powder, do not influence simultaneously weak activated rosin flux, particularly non-halogen solder flux has strengthened the practicality of solder alloy to the rupture of membranes reaction of alloy powder.
(2) adding of Sb has improved the wettability of solder alloy; Make follow-up application become more convenient.
(3) the precious metals ag content in the lead-free solder is reduced significantly, and cost descends significantly.With the 2010-10-15 metallic valence is example: the SAC305 material cost is 313 yuan/Kg, and SACGe (scolder of the present invention) material cost is 176 yuan/Kg.Cost descends 43.7%.
The specific embodiment:
Embodiment 1: each component is respectively by weight percentage: Ag 0.05%, and Cu 0.05%, Sb0.05%, and Ge 0.005%, and surplus is Sn.
Take by weighing 99.95% refined tin (Sn) 97.25Kg, join in the stainless steel crucible furnace, be warming up to 350-400 ℃, add 5% tin silver (Sn-Ag) intermediate alloy 1Kg, 10% tin copper (Sn-Cu) intermediate alloy 0.5Kg, 5% tin antimony (Sn-Sb) intermediate alloy 1Kg, 2% tin germanium (Sn-Ge) the intermediate alloy 0.25Kg that has prepared one by one, stirred energetically 10 minutes, leave standstill insulation 30 minutes, stirred 5 minutes, scrape off surface scum, tapping casting becomes the alloy bar of SnAg0.05Cu0.05Sb0.05Ge0.005.Wherein 50Kg makes the alloyed powder of 25-45um (No. 3) with the ultrasonic atomizatio method, physicochemical property and application performance after measuring its oxygen content and being made into soldering paste; All the other are used to measure the physicochemical property and the burn out rate of alloy.
Embodiment 2: each component is respectively by weight percentage: Ag0.05%, and Cu0.1%, Sb0.1%, Ge0.1%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.05Cu0.1Sb0.1Ge0.1, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 3: each component is respectively by weight percentage: Ag0.1%, and Cu0.25%, Sb0.05%, Ge0.005%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.1Cu0.25Sb0.05Ge0.005, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 4: each component is respectively by weight percentage: Ag0.25%, and Cu0.3%, Sb0.10%, Ge0.03%, surplus is Sn
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.25Cu0.3Sb0.1Ge0.03, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 5: each component is respectively by weight percentage: Ag0.3%, and Cu0.7%, Sb0.1%, Ge0.0075%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.3Cu0.7Sb0.1Ge0.0075, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 6: each component is respectively by weight percentage: Ag0.3%, and Cu0.8%, Sb0.16%, Ge0.047%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.3Cu0.8Sb0.16Ge0.047, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 7: each component is respectively by weight percentage: Ag0.5%, and Cu0.1%, Sb0.05%, Ge0.005%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.5Cu0.1Sb0.05Ge0.005, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 8: each component is respectively by weight percentage: Ag0.5%, and Cu0.1%, Sb0.2%, Ge0.021%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.5Cu0.1Sb0.2Ge0.021, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 9: each component is respectively by weight percentage: Ag0.75%, and Cu0.05%, Sb0.27%, Ge0.05%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.75Cu0.05Sb0.27Ge0.05, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 10: each component is respectively by weight percentage: Ag0.75%, and Cu0.7%, Sb0.50%, Ge0.10%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.75Cu0.7Sb0.5Ge0.01, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 11: each component is respectively by weight percentage: Ag0.8%, and Cu1.0%, Sb0.20%, Ge0.005%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg0.8Cu1.0Sb0.2Ge0.005, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 12: each component is respectively by weight percentage: Ag1.0%, and Cu0.1%, Sb0.05%, Ge0.075%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg1.0Cu0.1Sb0.05Ge0.075, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 13: each component is respectively by weight percentage: Ag1.0%, and Cu0.5%, Sb0.38%, Ge0.074%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg1.0Cu0.5Sb0.38Ge0.074, measure its physicochemical property and application performance according to the method for embodiment 1.
Embodiment 14: each component is respectively by weight percentage: Ag1.0%, and Cu1.0%, Sb0.5%, Ge0.1%, surplus is Sn.
Take by weighing quantitative refined tin and four kinds of intermediate alloys on request, make alloy bar and the alloyed powder of SnAg1.0Cu1.0Sb0.5Ge0.1, measure its physicochemical property and application performance according to the method for embodiment 1.
Now the fusing point and the rate of spread (standard solder flux) with traditional lead-free solder (SAC305, SAC0307) and the foregoing description 1-14 alloy compares (seeing Table 1):
Table 1: the contrast of the embodiment of the invention and traditional Sn-Ag-Cu lead-free solder
Table 2: the contrast of the embodiment of the invention and traditional Sn-Ag-Cu lead-free solder
Can find out from experimental data, add the liquidus temperature that a small amount of Ag can reduce solder alloy; Because the adding of metal Sb and Ge, solder wettability is improved; Can obviously reduce the burn out rate of alloy again, promptly improve the non-oxidizability of alloy; Simultaneously, also can reduce oxygen content after alloy is made glass putty.
The present invention is not limited to above-mentioned case study on implementation.In actual application, can select the alloying component in above-mentioned each case study on implementation according to the use occasion of different performance requirements, the perhaps heterogeneity proportioning except that above-mentioned case study on implementation, but all be no more than the scope of claims of the present patent application.
Claims (9)
1. the leadless welding alloy with oxidation resistance of a suitable powder process.It is characterized in that composed of the following components by weight percentage: Ag0.05-1.0%, Cu0.05-1.0%, Sb0.05-0.5%, Ge0.005-0.1%, surplus is Sn.
2. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 1 is characterized in that Ag content is 0.25-0.80%.
3. according to the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 2, it is characterized in that Ag content is 0.75%.
4. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 1 is characterized in that Cu content is 0.05-0.80%.
5. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 4 is characterized in that Cu content is 0.05%.
6. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 1 is characterized in that Sb content is 0.16-0.38%.
7. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 6 is characterized in that Sb content is 0.27%.
8. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 1 is characterized in that Ge content is 0.021-0.074%.
9. the leadless welding alloy with oxidation resistance of a kind of suitable powder process according to claim 8 is characterized in that Ge content is 0.047%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243234A (en) * | 2013-04-27 | 2013-08-14 | 深圳市同方电子新材料有限公司 | Serial low-silver and lead-free solder for electronic packaging soft soldering and preparation method thereof |
| CN105103279A (en) * | 2013-05-10 | 2015-11-25 | 富士电机株式会社 | Semiconductor device and method for manufacturing semiconductor device |
| CN105397330A (en) * | 2015-12-30 | 2016-03-16 | 上海新阳半导体材料股份有限公司 | Lead-free solder with high-temperature aging resistance and high strength |
| CN108941969A (en) * | 2018-07-20 | 2018-12-07 | 广东中实金属有限公司 | A kind of lead-free solder and preparation method thereof suitable for varistor |
| CN108971441A (en) * | 2018-07-13 | 2018-12-11 | 广东省材料与加工研究所 | A kind of supersonic casting method preparing hypereutectic high-temp leadless Sn-Cu solder ingot |
| CN110102931A (en) * | 2019-05-29 | 2019-08-09 | 华南理工大学 | A kind of improved microelectronics Packaging low silver Sn-Ag-Cu solder and preparation method thereof |
| CN111421260A (en) * | 2020-04-07 | 2020-07-17 | 威海新佳电子有限公司 | Solder alloy and preparation method thereof |
| CN112322929A (en) * | 2020-10-28 | 2021-02-05 | 云南锡业集团（控股）有限责任公司研发中心 | Intermediate alloy for improving oxidation resistance of solder |
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| US6179935B1 (en) * | 1997-04-16 | 2001-01-30 | Fuji Electric Co., Ltd. | Solder alloys |
| CN101007373A (en) * | 2006-12-04 | 2007-08-01 | 云南锡业集团（控股）有限责任公司 | Lead-free welding flux alloy |
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| US6179935B1 (en) * | 1997-04-16 | 2001-01-30 | Fuji Electric Co., Ltd. | Solder alloys |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243234A (en) * | 2013-04-27 | 2013-08-14 | 深圳市同方电子新材料有限公司 | Serial low-silver and lead-free solder for electronic packaging soft soldering and preparation method thereof |
| CN105103279A (en) * | 2013-05-10 | 2015-11-25 | 富士电机株式会社 | Semiconductor device and method for manufacturing semiconductor device |
| CN105103279B (en) * | 2013-05-10 | 2018-03-23 | 富士电机株式会社 | The manufacture method of semiconductor device and semiconductor device |
| CN105397330A (en) * | 2015-12-30 | 2016-03-16 | 上海新阳半导体材料股份有限公司 | Lead-free solder with high-temperature aging resistance and high strength |
| CN108971441A (en) * | 2018-07-13 | 2018-12-11 | 广东省材料与加工研究所 | A kind of supersonic casting method preparing hypereutectic high-temp leadless Sn-Cu solder ingot |
| CN108941969A (en) * | 2018-07-20 | 2018-12-07 | 广东中实金属有限公司 | A kind of lead-free solder and preparation method thereof suitable for varistor |
| CN110102931A (en) * | 2019-05-29 | 2019-08-09 | 华南理工大学 | A kind of improved microelectronics Packaging low silver Sn-Ag-Cu solder and preparation method thereof |
| CN111421260A (en) * | 2020-04-07 | 2020-07-17 | 威海新佳电子有限公司 | Solder alloy and preparation method thereof |
| CN111421260B (en) * | 2020-04-07 | 2022-04-19 | 威海新佳电子有限公司 | Solder alloy and preparation method thereof |
| CN112322929A (en) * | 2020-10-28 | 2021-02-05 | 云南锡业集团（控股）有限责任公司研发中心 | Intermediate alloy for improving oxidation resistance of solder |
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Application publication date: 20110330 |