CN101077553A - Sn-Ag-Cu-Ce leadless solder alloy and preparation method thereof - Google Patents
Sn-Ag-Cu-Ce leadless solder alloy and preparation method thereof Download PDFInfo
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- CN101077553A CN101077553A CN 200710017991 CN200710017991A CN101077553A CN 101077553 A CN101077553 A CN 101077553A CN 200710017991 CN200710017991 CN 200710017991 CN 200710017991 A CN200710017991 A CN 200710017991A CN 101077553 A CN101077553 A CN 101077553A
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Abstract
The present invention discloses one kind of no-lead Sn-Ag-Cu brazing alloy and its preparation process. The Sn-Ag-Cu brazing alloy consists of Ag 2.5-3.5 wt%, Cu 2.5-3.0 wt%, Ce 0.01-0.1 wt%, and Sn for the rest. Of the Sn-Ag-Cu brazing alloy, Cu can raise the welding performance and improve the plasticity of the alloy, Ce can raise the moistening capacity of the molten brazing alloy, and Ag can raise the mechanical performance and anticorrosive process of the alloy. Therefore, the no-lead Sn-Ag-Cu brazing alloy has high welding performance, high corrosion resistance and excellent mechanical performance, and may be used as electronic packing material.
Description
Technical field
The invention belongs to welding technology field, relate to a kind of Sn-Ag-Cu-Ce lead-free solder alloy, also relate to the preparation method of this kind Sn-Ag-Cu-Ce lead-free solder alloy.
Background technology
The Sn-Ag-Cu series leadless solder is acknowledged as and replaces one of the most promising solder of Sn-Pb solder.Its solder alloy fusion temperature scope is near 217 ℃, and melting temperature is higher, and good ductility is arranged, the outward appearance light.It has following several respects advantage: (1) fatigue durability is better than the Sn-Pb eutectic solder significantly; (2) tensile strength, early strength and long-term strength change all superior than Sn-Pb eutectic solder; Characteristics such as (3) to have deformation velocity slow in creep, and rupture time is long; (4) ductility descends ductility to some extent owing to add the metal that reduces fusing point, but does not have long-term deterioration problem; (5) good mechanical properties, good weldability.Though the Sn-Ag-Cu series leadless solder exists many advantages, also exist fusing point too high, therefore weak point such as wettability is poor, and cost is bigger has limited its application on industrial production.
Summary of the invention
The objective of the invention is, a kind of Sn-Ag-Cu-Ce lead-free solder alloy is provided, it is too high to solve Sn-Ag-Cu series leadless solder fusing point, the problem that cost is bigger.
Another object of the present invention provides the preparation method of this Sn-Ag-Cu-Ce lead-free solder alloy.
A technical scheme of the present invention is, a kind of Sn-Ag-Cu-Ce lead-free solder alloy, and composed of the following components by weight percentage: Ag is 2%～3%, and Cu is 2.5%～3%, and Ce is 0.01%～0.1%, and all the other are Sn, the weight sum of each component is 100%.
Alloy of the present invention, its component Ag purity is 99.99%.
Alloy of the present invention, its component Cu purity is 99.99%.
Alloy of the present invention, the purity of its component Ce is 99%.
Alloy of the present invention, its component S n is a cloud tin.
Another technical scheme of the present invention is, the preparation method of described Sn-Ag-Cu-Ce lead-free solder alloy carries out according to following steps,
With LiCl and KCl according to 1.0～1.2: 1.0～1.5 mass ratio takes by weighing respectively, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. take by weighing Ag 2%～3%, Cu 2.5%～3%, Rare-Earth Ce 0.01%～0.1% by mass ratio respectively, all the other are Sn, gross weight 100%, and put into corundum crucible and mix, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 450 ℃～700 ℃, be incubated 70 minutes～100 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 300 ℃～500 ℃, be incubated 40 minutes～60 minutes, stirs, and is cast into ingot at last again, promptly.
The invention has the beneficial effects as follows the cost that has reduced lead-free solder alloy, wettability is good, the mechanical property excellence.
Description of drawings
Fig. 1 is that alloy of the present invention welds, the micro-organization chart of its interface;
Fig. 2 is the DSC curve map of alloy of the present invention;
Fig. 3 is the stress strain curve figure of alloy of the present invention;
Fig. 4 is the fracture pattern and the micro-organization chart of alloy of the present invention.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Sn-Ag-Cu-Ce lead-free solder alloy of the present invention, composed of the following components by weight percentage: Ag is 2%～3%, Cu is 2.5%～3%, Ce is 0.01%～0.1%, all the other are Sn, and the weight sum of each component is 100%, and wherein component Ag purity is 99.99%, the purity of component Ce is 99%, and component S n is a cloud tin.
The Ag element can improve the mechanical performance and the corrosion resistance of alloy.When surpassing certain a certain amount of content, can reduce Sn-Ag-Cu is the liquidus curve of scolder.For making Ag and Cu, Sn formation eutectic or nearly eutectic form guarantee that to reduce welding temperature electronic component is not impaired, the content of Ag is controlled at 2～3%, cross to make the liquidus temperature rising at most, and Ag can increase production cost as noble metal; Form Ag
3The Sn particle can be strengthened matrix.Ag can also improve electrical conductivity in addition.
The Cu element can improve the alloy welding performance, and the plastic property to alloy also has improvement simultaneously; Formed Cu
6Sn
5Intermetallic compound particles is distributed on the tin matrix, plays invigoration effect.
Control the wettability of the scolder Ce element addition can increase fusing in a certain scope after, overcome the shortcoming of the wetability deficiency of some lead-free solder.In the alloy melting process, play catharsis, impel grain refinement, guarantee weld strength as the particle of heterogeneous body forming core crystallization.The fusing point of Ce own is low, can not improve welding temperature.The addition of considering Ce from the economy angle can not be too much.
Sn is a base-material, and Sn has low melting point, and the alloy that forms with other low-melting-point metal also just has relatively low fusing point, avoids thermal ablation or the fire damage of welding process for electronic devices and components.The Sn source is abundant, cheap, is various electronic package materials scolder base material.
The preparation method of Sn-Ag-Cu-Ce lead-free solder alloy of the present invention, carry out according to the following steps:
With LiCl and KCl according to 1.0～1.2: 1.0～1.5 mass ratio takes by weighing respectively, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. take by weighing Ag 2%～3%, Cu 2.5%～3%, Rare-Earth Ce 0.01%～0.1% by mass ratio respectively, all the other are Sn, gross weight 100%, all putting into corundum crucible mixes, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 450 ℃～700 ℃, be incubated 70 minutes～100 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 300 ℃～500 ℃, be incubated 40 minutes～60 minutes, stirs, and is cast into ingot at last again, promptly.
Embodiment one:
1. LiCl and KCl are taken by weighing respectively according to 1.1: 1.4 mass ratio, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. weighing sample, wherein the quality of Ag, Cu, Ce is respectively 2.0g (2%), 3.0g (3%), 0.05g (0.05%), all the other are Sn, total amount 100%, quality is total up to 100g, all putting into corundum crucible mixes, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 700 ℃, be incubated 90 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 400 ℃, be incubated 40 minutes, stirs, and is cast into ingot at last again, promptly.
The ingot that casting is good carries out specimen preparation, and its various aspects of performance is detected.219.7 ℃ of alloy melting points, solder joint light, spreading area 201.6mm
2(the Sn37Pb alloy is 236.5mm under the same terms
2), microscopic structure is tiny and uniform eutectic structure, and tensile strength is 36.46MPa, and percentage elongation is 11.3%, and welding point is at 50 ℃, and load is under the 8.75MPa condition, and be 98 hours creep life.
Embodiment two:
1. LiCl and KCl are taken by weighing respectively according to 1.0: 1.0 mass ratio, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. weighing sample, wherein the quality of Ag, Cu, Ce is respectively 2.5g (2.5%), 2.8g (2.8%), 0.1g (0.1%), all the other are Sn, total amount 100%, quality is total up to 100g, all putting into corundum crucible mixes, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 450 ℃, be incubated 70 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 500 ℃, be incubated 50 minutes, stirs, and is cast into ingot at last again, promptly.
The ingot that casting is good carries out specimen preparation, and its various aspects of performance is detected.218.8 ℃ of alloy melting points, solder joint light, spreading area 220.6mm
2(the Sn37Pb alloy is 236.5mm under the same terms
2), microscopic structure is tiny and uniform eutectic structure, and tensile strength is 38.24MPa, and percentage elongation is 13.6%, and welding point is at 50 ℃, and load is under the 8.75MPa condition, and be 124 hours creep life.
Embodiment three:
1. LiCl and KCl are taken by weighing respectively according to 1.2: 1.5 mass ratio, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. the quality of wherein Ag, the Cu of weighing sample, Ce is respectively 3.0g (3%), 3.0g (3%), 0.01g (0.01%), and all the other are Sn.Total amount 100%, quality is total up to 100g, all putting into corundum crucible mixes, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 600 ℃, be incubated 100 minutes, stirred once in per during this period 10 minutes, and after melting is intact crucible was taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 300 ℃, be incubated 60 minutes, stirs, and is cast into ingot at last again, promptly.
The ingot that casting is good carries out specimen preparation, and its various aspects of performance is detected.220.3 ℃ of alloy melting points, solder joint light, spreading area 207.3mm
2(the Sn37Pb alloy is 236.5mm under the same terms
2), microscopic structure is tiny and uniform eutectic structure, and tensile strength is 40.58MPa, and percentage elongation is 15.7%, and welding point is at 50 ℃, and load is under the 8.75MPa condition, and be 85 hours creep life.
Embodiment four:
1. LiCl and KCl are taken by weighing respectively according to 1.0: 1.0 mass ratio, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
2. weighing sample, wherein the quality of Ag, Cu, Ce is respectively 2.5g (2.5%), 2.5g (2.5%), 0.1g (0.1%), all the other are Sn, total amount 100%, quality is total up to 100g, all putting into corundum crucible mixes, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 450 ℃, be incubated 70 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
3. the alloy that above-mentioned casting is good carries out remelting under 500 ℃, be incubated 50 minutes, stirs, and is cast into ingot at last again, promptly.
The ingot that casting is good carries out specimen preparation, and its various aspects of performance is detected.218.8 ℃ of alloy melting points, solder joint light, spreading area 220.6mm
2(the Sn37Pb alloy is 236.5mm under the same terms
2), microscopic structure is tiny and uniform eutectic structure, and tensile strength is 38.24MPa, and percentage elongation is 13.6%, and welding point is at 50 ℃, and load is under the 8.75MPa condition, and be 124 hours creep life.
Fig. 1 is that alloy of the present invention welds, the micro-organization chart of its interface; Show that weld structure is very even, the formed second phase particle particle is tiny, can play good tough effect, improves the weld strength and the soldering reliability of alloy, satisfies the pb-free solder requirement.
Fig. 2 is the DSC curve map of alloy of the present invention; The fusing point that shows this solder is less than the desired requirement that is lower than 220 ℃ of pb-free solder.
Fig. 3 is the stress strain curve figure of alloy of the present invention; Show that this solder has suitable extensibility under certain load, help the connection of components and parts.
Fig. 4 is the fracture pattern and the micro-organization chart of alloy of the present invention.Its tension failure face is that fibrous pattern shows that this solder of this solder fracture mode is non-brittle fracture.This also is one of this scolder major reason that good welds intensity and practical value are arranged.
In sum, Pb-free solder alloy cost of the present invention is lower, and wettability is good, and its spreading area can reach 89% of traditional Sn37Pb alloy, and alloy melting point is 218.8-220.3 ℃, and the mechanical property excellence can be used as electronic package material and is extensive use of.
Claims (6)
1. Sn-Ag-Cu-Ce lead-free solder alloy, it is characterized in that: composed of the following components by weight percentage: Ag is 2%～3%, and Cu is 2.5%～3%, and Ce is 0.01%～0.1%, and all the other are Sn, the weight sum of each component is 100%.
2. alloy as claimed in claim 1 is characterized in that: its component Ag purity is 99.99%.
3. alloy as claimed in claim 1 is characterized in that: its component Cu purity is 99.99%.
4. alloy as claimed in claim 1 is characterized in that: the purity of its component Ce is 99%.
5. alloy as claimed in claim 1 is characterized in that: its component S n is a cloud tin.
6. method for preparing the described alloy of claim 1, it is characterized in that: this method is carried out according to the following steps,
A. with LiCl and KCl according to 1.0～1.2: 1.0～1.5 mass ratio takes by weighing respectively, and load weighted LiCl and KCl are mixed, the preparation fused salt that is protected;
B. take by weighing Ag 2%～3%, Cu 2.5%～3%, Rare-Earth Ce 0.01%～0.1% by mass ratio respectively, all the other are Sn, gross weight 100%, and put into corundum crucible and mix, the above-mentioned protection fused salt for preparing is covered on the mixture in the crucible, put into resistance furnace and heat melting, when treating that temperature reaches 450 ℃～700 ℃, be incubated 70 minutes～100 minutes, stirred once in per during this period 10 minutes, after melting is intact crucible is taken out, the alloy in the crucible is carried out precooling, casting;
C. above-mentioned casting is good alloy carries out remelting under 300 ℃～500 ℃, be incubated 40 minutes～60 minutes, stirs, and is cast into ingot at last again, promptly.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381826B (en) * | 2008-09-26 | 2012-11-07 | 南昌大学 | Sn-Cu base leadless solder alloy and preparation method |
| CN103056543A (en) * | 2013-01-18 | 2013-04-24 | 江苏师范大学 | Lead-free nanometer solder containing Yb, A1 and B |
| CN103862189A (en) * | 2014-03-10 | 2014-06-18 | 北京控制工程研究所 | Soft solder for welding gold or gold alloy and preparation method thereof |
| CN111705239A (en) * | 2020-06-29 | 2020-09-25 | 泰安晶品新材料科技有限公司 | Material formula and smelting process of BGA solder balls for packaging integrated circuit |
| CN112342417A (en) * | 2020-11-17 | 2021-02-09 | 昆明理工大学 | Tin-based solder and preparation method thereof |
| CN113182727A (en) * | 2021-04-08 | 2021-07-30 | 北京科技大学 | Chlorine ion corrosion resistant Sn-Ag-Cu-Nd lead-free solder alloy and preparation method thereof |
| CN113458650A (en) * | 2021-07-05 | 2021-10-01 | 云南锡业锡材有限公司 | Sn-Ag-Cu-Ce high-reliability lead-free solder |
| CN114289927A (en) * | 2021-12-28 | 2022-04-08 | 上海大学 | Lead-free solder |
| CN114559179A (en) * | 2022-03-31 | 2022-05-31 | 昆明理工大学 | Sn-Ag-Cu low-melting-point lead-free solder and preparation method thereof |
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2007
- 2007-06-05 CN CN 200710017991 patent/CN101077553A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381826B (en) * | 2008-09-26 | 2012-11-07 | 南昌大学 | Sn-Cu base leadless solder alloy and preparation method |
| CN103056543A (en) * | 2013-01-18 | 2013-04-24 | 江苏师范大学 | Lead-free nanometer solder containing Yb, A1 and B |
| CN103056543B (en) * | 2013-01-18 | 2015-03-25 | 江苏师范大学 | Lead-free nanometer solder containing Yb, A1 and B |
| CN103862189A (en) * | 2014-03-10 | 2014-06-18 | 北京控制工程研究所 | Soft solder for welding gold or gold alloy and preparation method thereof |
| CN103862189B (en) * | 2014-03-10 | 2016-08-17 | 北京控制工程研究所 | A kind of soft solder for welding gold or billon and preparation method thereof |
| CN111705239A (en) * | 2020-06-29 | 2020-09-25 | 泰安晶品新材料科技有限公司 | Material formula and smelting process of BGA solder balls for packaging integrated circuit |
| CN112342417A (en) * | 2020-11-17 | 2021-02-09 | 昆明理工大学 | Tin-based solder and preparation method thereof |
| CN112342417B (en) * | 2020-11-17 | 2022-03-15 | 昆明理工大学 | Tin-based solder and preparation method thereof |
| CN113182727A (en) * | 2021-04-08 | 2021-07-30 | 北京科技大学 | Chlorine ion corrosion resistant Sn-Ag-Cu-Nd lead-free solder alloy and preparation method thereof |
| CN113458650A (en) * | 2021-07-05 | 2021-10-01 | 云南锡业锡材有限公司 | Sn-Ag-Cu-Ce high-reliability lead-free solder |
| CN114289927A (en) * | 2021-12-28 | 2022-04-08 | 上海大学 | Lead-free solder |
| CN114559179A (en) * | 2022-03-31 | 2022-05-31 | 昆明理工大学 | Sn-Ag-Cu low-melting-point lead-free solder and preparation method thereof |
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