CN101439444A - Low tin-zinc base leadless metal spraying solder - Google Patents
Low tin-zinc base leadless metal spraying solder Download PDFInfo
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- CN101439444A CN101439444A CNA2008101878554A CN200810187855A CN101439444A CN 101439444 A CN101439444 A CN 101439444A CN A2008101878554 A CNA2008101878554 A CN A2008101878554A CN 200810187855 A CN200810187855 A CN 200810187855A CN 101439444 A CN101439444 A CN 101439444A
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Abstract
The invention relates to a low-tin-zinc-base lead-free metal spraying solder. The solder alloy comprises the following components by parts by weight: 1-10 parts of Sn, 0.1-4 parts of Al, 0.01-0.5 part of Si, 0.1-1 parts of Cu, 0.08-1.2 parts of Sb, 0.01-0.5 part of Pd, 0.001-0.01 part of Nd and 82-98 parts of Zn. The metal spraying solder of the invention has strong oxidation resistance in high temperature, excellent wetting property, reliable welding and better conductivity and mechanical property than lead-base metal spraying solder. Main performance indexes and application effect of the solder completely reach and surpass level of existing lead-free metal spraying solder, thereby overcoming the high-cost defect of lead-free metal spraying solder; the solder also avoids lead poisoning caused by leaded metal spraying solder.
Description
Technical field
The present invention relates to a kind of low tin-zinc base leadless metal spraying solder, relate in particular to a kind of low tin-zinc base leadless metal spraying solder that is applicable to MMB end face spraying in the electric discrete device, belong to electronic technology material and electronics preparing technical field.
Background technology
The conductive material that the lead base gold-spraying solder sprays as the thin film capacitor end face for a long time, because of having many excellent properties, in electronics industry, once accounting for leading position, but lead has toxicity, when waste electronic electrical equipment landfill disposal, lead in the scolder is met acid rain or underground water forms leaded salt, be soluble in underground water, enter human water supply chain, and enter in the human body, accumulating over a long period to cause lead poisoning, and the back lead of poisoning is difficult for getting rid of external again.And the lead base gold-spraying solder in use, also can bring great harm to the operator.And general its primary raw material of no lead base gold-spraying solder commonly used at present is precious metal Sn (tin), its content is the highest can be reached more than 90%, though can substitute poisonous leaded gold-spraying solder in technical indicator and practical art aspect of performance, its cost is too high, and is unfavorable for extensive use.
Summary of the invention
The objective of the invention is to propose a kind of low tin-zinc base leadless metal spraying solder and preparation method thereof, a kind of low tin-zinc base leadless metal spraying solder that is applicable to metallic film capacitor end face spraying in the electrical equipment discrete device especially is provided, it is strong that this gold-spraying solder possesses under the high temperature oxidation resistance, wetability is good, welding is reliable, electric conductivity and mechanical property are better than the lead base gold-spraying solder, and its main performance index and effect reach and surmount the level of existing no lead base gold-spraying solder fully.Overcome the leadless gold-spraying solder defect of high cost, and had plumbous gold-spraying solder to cause saturnine bad phenomenon easily.
The objective of the invention is to be achieved through the following technical solutions:
A kind of low tin-zinc base leadless metal spraying solder, the weight portion of each chemical raw material is Sn1-10, Al 0.1-4, Si 0.01-0.5, Cu 0.1-1, Sb 0.08-1.2, Pd 0.01-0.5, Nd 0.001-0.01 in the described solder alloy, Zn 82-98;
The weight portion of each chemical raw material is preferably Sn 3-9, Al 0.2-3.5, Si0.04-0.4, Cu 0.2-0.8, Sb 0.09-1.1, Pd 0.04-0.4, Nd 0.004-0.007, Zn84-96 in the described solder alloy;
The present invention also provides a kind of preparation method of low tin-zinc base leadless metal spraying solder, may further comprise the steps:
(1), by weight take by weighing above-mentioned various raw material, and, put into container, heat fused the Sn that weighs up;
(2), be that the lithium chloride of 1:1 and potassium chloride mix as coverture with weight ratio, cover on the Sn liquid level of fusing, make the oxygen in the Sn liquid level secluding air;
(3), when Sn liquid is warming up to 900 ± 50 ℃, add Al, Si, Cu, Sb, Pd, Nd successively, heat while stirring.To quicken fusing, treat all fusings after, stop heating, leave standstill 25-35 minute after, remove the mixing coverture, ingot casting is the many first intermediate alloys of SnASiCuSbPdNd;
(4), Zn is placed another container, add above-mentioned coverture after, heating makes the Zn fusing, and add the polynary intermediate alloy of (3) preparation when its temperature risen to 600 ± 50 ℃, and stir and make the intermediate alloy fusing, be dispersed in the Zn liquid, stop heating, left standstill 25-35 minute;
(5) remove coverture, alloy is gone out container solidify and promptly get described low tin-zinc base leadless metal spraying solder.
The present invention is that fusing point is low after forming alloy based on the gold-spraying solder of Zn and Sn, intensity height, and the price of Zn is low, and totle drilling cost descends greatly, but Zn is more active metallic element, corrosion resistance is poor, especially at high temperature very easily oxidation and influence solderability.When in the ZnSn alloy, adding the Al of 0.1%-4%; Al can form fine and close indifferent oxide protective layer at alloy surface; improved the anti-oxidant corrosion resistance of ZnSN alloy; the ductility of Al is good again; make the ZnSnAl alloy be convenient to processing; the cost of Al is also lower; but the fusing point of Al is about 660 ℃; the fusing point that adds affiliation raising ZnSnAl alloy of Al; but its molten temperature region broadens; this will cause the viscosity of ZnSnAl alloy to increase, and wettability reduces, therefore on the basis that adds Al; add a kind of hard and smooth again; metalloid element crystal Si with semiconducting behavior adjusts, and its optimum amount is 0.01-0.5%, and this will reduce the fusing point and the viscosity of alloy significantly; and do not produce fragility; the effect that reduces the scolder fusing point when consumption is lower than 0.01% is not obvious, and greater than the electric conductivity that influenced scolder at 0.05% o'clock again, conductance is on a declining curve.In order to improve the wetability of ZnSnAlSi alloy, guarantee reliable welding performance, add The addition of C u.Cu and Zn can generate the ZnCu intermetallic compound again, when the addition of Cu can reduce the Zn element gradually at the melting solder surface oxidation during for 0.1%-1%, significantly lower the surface tension of melt scolder, reduce scolder and the contact angle that is welded the position, improve the wetting state of scolder, thereby improve the solderability of scolder greatly.When Cu content is lower than 0.1%, wetting effect is not obvious, and the Cu addition reaches at 1% o'clock, and the non-oxidizability of alloy and wetability are best again, but when addition greater than 0.7% the time, because the intermetallic compound that generates too much can make the scolder ductility that becomes fragile influenced again.Add an amount of quality softness have good ductility and plastic Pd element in alloy in order to solve this defective, revise, the adding of Pd has also improved the electric conductivity of alloy under the low current greatly.The stretching and the shear strength that add suitable Sb butt welding point in the scolder are very favourable, and optimum amount is 0.08%-1.2%
Zn is the major metal raw material in this solder, Zn and Sn, Al, Si, Cu, Sb, Pd.The multicomponent alloy scolder that each metal or metalloid element form has anti-oxidant, and decay resistance is strong, and wetability is good, the excellent electrical properties that solderability is high.But the heterogeneous microstructure of solder and mechanical property are desirable not enough, the characteristic property of rare earth element can change the combination property of alloy effectively, in existing rare earth element, show that the raw material of lanthanum (La) is rare and valuablely be difficult for a large amount of buyings by application experiment.The adding of cerium (Ce) is that the atomic scolder that also can make of use amount is clamminess under melt, and flowability is also bad, stirs the melt scolder and quickens the oxidation of scolder on the contrary.Some other rare earth element also is unfavorable for welding process requirement after adding.The active rare earth element nd of trace not only is easy to accumulate in the interface and the surface of solder under liquid state, the surface of alloy can obviously be descended, increased with by the wetting power of sprayed surface, and refinement the metallographic structure of solder, the mechanical property of having improved solder has improved ductility and shear strength.Its best 0.001%-0.01% that uses
A kind of low tin-zinc base leadless metal spraying solder of the present invention has the following advantages:
1, The present invention be directed to leadless gold-spraying solder cost height, tradition lead base gold-spraying solder causes saturnine bad phenomenon easily, only adopt based on behind the metallic element formation alloys such as the gold-spraying solder of Zn and Sn, fusing point is low, the intensity height, and the price of Zn is low, thus totle drilling cost descends greatly, it is low to reach cost, the purpose that effect is good.
2, at high temperature oxidation resistance is strong for gold-spraying solder of the present invention, and wetability is good, and welding is reliable, and electric conductivity and mechanical property are better than the lead base gold-spraying solder, and its main performance index and effect reach fully and surmount in the level of existing no lead base gold-spraying solder.
In order to prove and assess the combination property of the low Sn zinc base leadless metal spraying solder of the present invention, implementing 8 schemes with embodiment 1-is proportioning, each is as a comparison case a kind of to have chosen the homemade Al of containing gold-spraying solder commonly used at present and leadless gold-spraying solder simultaneously, is respectively through its chemical raw material of atomic absorption spectrometry:
Contrast 1 leaded gold-spraying solder: Sn41%, Zn2.2%, Sb1.1%, BiO.4%, surplus Pb
Contrast 2 leadless gold-spraying solders: Sn68.2%, Sb1.2%CuO.37% surplus Zn,
Embodiment 1-embodiment 8 and Comparative Examples synthetic performance evaluation the results are shown in following table
| The gold-spraying solder sequence number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative Examples 1 | Comparative Examples 2 |
| Solidus temperature (℃) | 195 | 187 | 190 | 196 | 198 | 188 | 193 | 197 | 169 | 204 |
| Liquidus temperature (℃) | 411 | 390 | 407 | 405 | 400 | 403 | 406 | 401 | 341 | 367 |
| Shear strength (N/mm 2) | 164 | 172 | 187 | 195 | 157 | 162 | 159 | 173 | 64 | 151 |
| Elongation (%) | 39 | 47 | 41 | 49 | 43 | 39 | 42 | 47 | 33 | 37 |
| Resistivity (M Ω .mm 2/M·) | 72.9 | 77.3 | 78.2 | 75.1 | 74.2 | 70.4 | 79.2 | 70.3 | 131 | 82.4 |
| Wetability (%) | 82 | 81 | 83 | 82 | 81 | 81 | 84 | 80 | 80 | 79 |
| Dielectric loss rate 100KHZ | 1.39 | 1.41 | 1.43 | 1.38 | 1.42 | 1.46 | 1.50 | 1.46 | 1.51 | 1.69 |
| Non-oxidizability (slag yield) % | 3.5 | 3.7 | 3.2 | 3.3 | 3.1 | 3.2 | 3.1 | 3.0 | 2.9 | 4.1 |
Test data from table as can be seen the present invention to have non-oxidizability strong, high temperature is slagged tap few, and wetability is good, and mechanical strength is higher, creep-resistant property and electric property all are better than lead base and existing leadless gold-spraying solder like product, and cost of material is significantly less than existing leadless gold-spraying solder.
The specific embodiment
Embodiment 1
Raw material: (Kg) Sn 1, Al 0.8, Si 0.1, Cu 0.2, Sb 0.08, Pd 0.04, Nd 0.005, Zn 97
The preparation method:
(1), by weight percentage take by weighing various raw materials, and the Sn that weighs up is put into graphite crucible, heat fused earlier.
(2), be that the lithium chloride of 1:1 and potassium chloride mix as coverture with weight ratio, cover fully on the Sn liquid level of fusing, thickness is 3 millimeters, makes the oxygen in the Sn liquid level secluding air.
(3), when Sn liquid is warming up to 850 ℃, adds Al, Si, Cu, Sb, Pd, Nd, a kind of metal of every adding successively and all need stir with dry wooden stick.To quicken fusing, treat all fusings after, stop heating, leave standstill 25 minutes after, remove the mixing coverture, ingot casting is the many first intermediate alloys of SnAlSiCuSbPdNd
(4), Zn is placed another graphite crucible, add above-mentioned coverture after, heating makes the Zn fusing, and add the polynary intermediate alloy of (3) preparation when its temperature risen to 550 ℃, and stir with dry wooden stick intermediate alloy is melted, be dispersed in the Zn liquid, stop heating, left standstill 25 minutes.
(5) remove coverture, alloy is taken the dish out of the pot to solidify promptly gets described low tin-zinc base leadless metal spraying solder.
Embodiment 2
Raw material: (Kg) Sn 10, Al 4, Si 0.4, Cu 0.8, Sb 1, Pd 0.3, Nd 0.01, Zn 83
The preparation method:
(1), by weight take by weighing various raw materials, and, put into container, heat fused the Sn that weighs up;
(2), be that the lithium chloride of 1:1 and potassium chloride mix as coverture with weight ratio, cover on the Sn liquid level of fusing, make the oxygen in the Sn liquid level secluding air;
(3), when Sn liquid is warming up to 900 ℃, add Al, Si, Cu, Sb, Pd, Nd successively, heat while stirring.To quicken fusing, treat all fusings after, stop heating, leave standstill 30 minutes after, remove the mixing coverture, ingot casting is the many first intermediate alloys of SnAlSiCuSbPdNd;
(4), Zn is placed another container, add above-mentioned coverture after, heating makes the Zn fusing, and adds the polynary intermediate alloy of (3) preparation when its temperature risen to 600 ℃, stirs and makes the intermediate alloy fusing, is dispersed in the Zn liquid, stops heating, leaves standstill 30 minutes;
(5) remove coverture, alloy is gone out container solidify and promptly get described low tin-zinc base leadless metal spraying solder.
Embodiment 3
Raw material: (Kg) Sn 7, Al 2, Si 0.2, Cu 1, Sb 1.1, Pd 0.4, Nd 0.001, Zn 88
The preparation method:
(1), by weight take by weighing various raw materials, and, put into container, heat fused the Sn that weighs up;
(2), be that 1: 1 lithium chloride and potassium chloride mix as coverture with weight ratio, cover on the Sn liquid level of fusing, make the oxygen in the Sn liquid level secluding air;
(3), when Sn liquid is warming up to 950 ℃, add Al, Si, Cu, Sb, Pd, Nd successively, heat while stirring.To quicken fusing, treat all fusings after, stop heating, leave standstill 35 minutes after, remove the mixing coverture, ingot casting is the many first intermediate alloys of SnAlSiCuSbPdNd;
(4), Zn is placed another container, add above-mentioned coverture after, heating makes the Zn fusing, and adds the polynary intermediate alloy of (3) preparation when its temperature risen to 650 ℃, stirs and makes the intermediate alloy fusing, is dispersed in the Zn liquid, stops heating, leaves standstill 35 minutes;
(5) remove coverture, alloy is gone out container solidify and promptly get described low tin-zinc base leadless metal spraying solder.
Embodiment 4
Raw material: (Kg) Sn 5, Al 1, Si 0.04, Cu 0.2, Sb 1.2, Pd 0.01, Nd 0.003, Zn 92
The preparation method is with embodiment 1
Embodiment 5
Raw material: (Kg) Sn 9, Al 0.1, Si 0.01, Cu 0.1, Sb 0.09, Pd 0.5, Nd 0.007, Zn 90
The preparation method is with embodiment 1
Embodiment 6
Raw material: (Kg) Sn 8.5, Al 3.5, Si 0.34, Cu 0.7, Sb 1.05, Pd 0.35, Nd 0.004, Zn 85
The preparation method is with embodiment 1
Embodiment 7
Raw material: (Kg) Sn 1, Al 0.2, Si 0.3, Cu 0.6, Sb 1, Pd 0.4, Nd 0.006, Zn 96
The preparation method is with embodiment 1
Embodiment 8
Raw material: (Kg) Sn 3, Al 0.4, Si 0.4, Cu 0.5, Sb 1.2, Pd 0.2, Nd 0.01, Zn 94
The preparation method is with embodiment 1
Claims (3)
1, a kind of low tin-zinc base leadless metal spraying solder, the weight portion of each chemical raw material is Sn1-10, A1 0.1-4, Si 0.01-0.5, Cu 0.1-1, Sb 0.08-1.2, Pd 0.01-0.5, Nd 0.001-0.01 in the described solder alloy, Zn 82-98;
2, according to a kind of low tin-zinc base leadless metal spraying solder of claim 1, the weight portion of each chemical raw material is Sn 3-9, A1 0.2-3.5, Si 0.04-0.4, Cu 0.2-0.8, Sb0.09-1.1, Pd 0.04-0.4, Nd 0.004-0.007 in the described solder alloy, Zn 84-96;
3, the preparation method of a kind of low tin-zinc base leadless metal spraying solder of one of claim 1-2 may further comprise the steps:
(1), take by weighing various raw materials, and, put into container, heat fused the Sn that weighs up by one of claim 1-2 weight portion;
(2), be that the lithium chloride of 1:1 and potassium chloride mix as coverture with weight ratio, cover on the Sn liquid level of fusing, make the oxygen in the Sn liquid level secluding air;
(3), when Sn liquid is warming up to 900 ± 50 ℃, add Al, Si, Cu, Sb, Pd, Nd successively, heat while stirring.To quicken fusing, treat all fusings after, stop heating, leave standstill 25-35 minute after, remove the mixing coverture, ingot casting is the many first intermediate alloys of SnAlSiCuSbPdNd;
(4), Zn is placed another container, add above-mentioned coverture after, heating makes the Zn fusing, and add the polynary intermediate alloy of (3) preparation when its temperature risen to 600 ± 50 ℃, and stir and make the intermediate alloy fusing, be dispersed in the Zn liquid, stop heating, left standstill 25-35 minute;
(5) remove coverture, alloy is gone out container solidify and promptly get described low tin-zinc base leadless metal spraying solder.
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| CN102672367A (en) * | 2011-12-12 | 2012-09-19 | 河南科技大学 | ZnSn-base high-temperature lead-free soft solder and preparation method thereof |
| TWI381900B (en) * | 2009-08-06 | 2013-01-11 | Chenming Mold Ind Corp | Metal bonding structure and joining method thereof |
| CN103223560A (en) * | 2013-02-25 | 2013-07-31 | 重庆科技学院 | Lead-free brazing filler metal for replacing high-lead high-temperature brazing filler metal, and preparation method of lead-free brazing filler metal |
| CN105904115A (en) * | 2016-06-14 | 2016-08-31 | 福建工程学院 | ZnSn-based high-temperature lead-free soft solder and preparation method thereof |
| CN106238956A (en) * | 2016-08-30 | 2016-12-21 | 郑州机械研究所 | A kind of low melting point brazing material, preparation method and applications |
| CN106271191A (en) * | 2016-08-31 | 2017-01-04 | 郑州机械研究所 | A kind of green high-strength low temperature composite soldering and preparation method thereof |
| CN107627044A (en) * | 2017-10-25 | 2018-01-26 | 吉林大学 | The polynary zinc-tin copper bismuth neodymium solder and its preparation technology of a kind of soldering sintered NdFeB and steel |
| CN112296550A (en) * | 2020-10-13 | 2021-02-02 | 好利来（厦门）电路保护科技有限公司 | Zinc-based high-temperature lead-free soldering tin and production method thereof |
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2008
- 2008-12-24 CN CN2008101878554A patent/CN101439444B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI381900B (en) * | 2009-08-06 | 2013-01-11 | Chenming Mold Ind Corp | Metal bonding structure and joining method thereof |
| CN102672367A (en) * | 2011-12-12 | 2012-09-19 | 河南科技大学 | ZnSn-base high-temperature lead-free soft solder and preparation method thereof |
| CN102672367B (en) * | 2011-12-12 | 2015-05-13 | 河南科技大学 | ZnSn-base high-temperature lead-free soft solder and preparation method thereof |
| CN103223560A (en) * | 2013-02-25 | 2013-07-31 | 重庆科技学院 | Lead-free brazing filler metal for replacing high-lead high-temperature brazing filler metal, and preparation method of lead-free brazing filler metal |
| CN105904115A (en) * | 2016-06-14 | 2016-08-31 | 福建工程学院 | ZnSn-based high-temperature lead-free soft solder and preparation method thereof |
| CN105904115B (en) * | 2016-06-14 | 2018-07-10 | 福建工程学院 | A kind of ZnSn-base high-temperature lead-free soft solder and preparation method thereof |
| CN106238956A (en) * | 2016-08-30 | 2016-12-21 | 郑州机械研究所 | A kind of low melting point brazing material, preparation method and applications |
| CN106271191A (en) * | 2016-08-31 | 2017-01-04 | 郑州机械研究所 | A kind of green high-strength low temperature composite soldering and preparation method thereof |
| CN106271191B (en) * | 2016-08-31 | 2018-09-21 | 郑州机械研究所有限公司 | A kind of high-strength low temperature composite soldering of green and preparation method thereof |
| CN107627044A (en) * | 2017-10-25 | 2018-01-26 | 吉林大学 | The polynary zinc-tin copper bismuth neodymium solder and its preparation technology of a kind of soldering sintered NdFeB and steel |
| CN112296550A (en) * | 2020-10-13 | 2021-02-02 | 好利来（厦门）电路保护科技有限公司 | Zinc-based high-temperature lead-free soldering tin and production method thereof |
| CN112296550B (en) * | 2020-10-13 | 2022-07-26 | 好利来（厦门）电路保护科技有限公司 | Zinc-based high-temperature lead-free soldering tin and production method thereof |
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