CN109894769A - A kind of zinc-tin base leadless solder of high creep resistance and preparation method thereof - Google Patents
A kind of zinc-tin base leadless solder of high creep resistance and preparation method thereof Download PDFInfo
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- CN109894769A CN109894769A CN201910244999.7A CN201910244999A CN109894769A CN 109894769 A CN109894769 A CN 109894769A CN 201910244999 A CN201910244999 A CN 201910244999A CN 109894769 A CN109894769 A CN 109894769A
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Abstract
The present invention is a kind of zinc-tin base leadless solder and preparation method thereof of high creep resistance, it is less to provide a kind of alloy constituent element, it is convenient to smelt, easily controllable impurity lead content, wettability is good, shear strength with higher and suitable fusion temperature, and there is good plastic forming ability, and the lead-free high-temperature soft solder of creep-resistant property with higher.
Description
Technical field
The present invention relates to field of material technology, more particularly to the zinc-tin base leadless solder and its system of a kind of high creep resistance
Preparation Method.
Background technique
SnPb alloy is widely used in Electronic Packaging and surface mount SMT(Surface Mount Technology)
Technology.With 95Pb-5Sn.90Pb-l0Sn and 95.5Pb-2Sn-2.5Ag etc. for the w (Pb) 85% of representative high lead solder micro-
The high-temperature field of Electronic Packaging is widely used.Microelectronic component of the high lead solder not only to work under harsh thermal environment provides
It consolidates and reliably connects, high-melting-point alloy when being also brazed as step is used for the level package of electronic component, is large-scale
Information technoloy equipment and the military projects such as network infrastructure, large power supply and switch, automotive electronics, aerospace and the crucial electricity of civil field
Particularly important interconnection material in sub- equipment packages.
Under the guidance of WEEE/RoHS decree, various countries make laws in succession to limit the deleterious materials such as Pb in microelectronic industry
In use, intermediate temperature solder and low-temperature brazing filler metal have been carried out it is unleaded, but in view of suitable high-temp solder can not be found at present
Alternative materials, using RoHS as the regulation of representative to the use of the high lead solder of special-purpose in microelectronic industry give temporarily slit
Exempt from.
Lead-free brazing substitutes high lead solder and must meet the following requirement:
(1) solidus is higher than 260 DEG C (secondary backs for avoiding solder) and liquidus point will be lower than 400 DEG C (due to polymer matrix
The limitation of body glass transition temperature), and melting range small as far as possible；(2) lower modulus of shearing；(3) good thermal conductivity and
Lower resistance coefficient；(4) good inoxidizability；(5) good corrosion resistance；(6) good processing performance, can be made
Finished product of different shapes；(7) acceptable cost price；(8) non-toxic；(9) it is easy to exploit, rich reserves.
In terms of present Research both domestic and external, in candidate high-temp leadless brazing filler metal alloy system, have Au-Sn, Zn-Al, Bi-Ag,
The binary alloy systems such as Sn-Sb, Zn-Sn.Practical lead-free high-temperature soft solder is mainly Au based alloy at present, intensity is high,
Conductive and excellent heat conductivity, but it is more crisp, and elongation percentage is smaller, and not easy to be processed at various shape, stress relaxation ability is poor.This
Outside, since Au is expensive, it is served only for high-end field.
Japanese Patent Laid-Open 2014-151364, proposes Zn-(6-8) In solder and be added on this basis 5%Al or
The brazing filler metal alloy that person 0.1%Ge or a small amount of Bi are characterized.But contain indium in the alloy, abundance of the In in the earth's crust is very low, and price
Valuableness is not suitable for large-scale use.Chinese patent CN102672367A proposes Zn base high-temperature leadless soft solder by following weight
Percentage composition at being grouped as: 15-40% tin, 0.5-8%Cu, 0.1-1% lanthanum neodymium mixed rare-earth, 0.1-3%Mg, 0.1-2%Bi are remaining
Amount is Zn.But alloy constituent element is more, practicability is poor.Chinese patent CN102554491A proposes Zn base high-temperature leadless soft solder
By following weight percentage at being grouped as: the aluminium of 2-30%, the tin of 1-20%, the copper of 0.1-8%, 0.01-3.0%'s
Titanium, the manganese of 0.1-1.0% and/or the lanthanum cerium mischmetal of 0.1-1.0%, the zinc of surplus.But the strength of alloy improves, alloy
Plastic forming ability reduces.Chinese patent CN101380701A proposes Bi-based high temperature lead-free brazing, and material component is by weight
It is calculated as: 2-8% antimony；2-12% tin, 0.5-5% copper, remaining is bismuth.But the brittleness of Bi is very big.In addition, Bi is the pair of lead
Product must increase the exploitation to lead ore using the solder containing Bi, cause the pollution to environment.Chinese patent
CN105904115B proposes Zn base high-temperature leadless soft solder by following weight percentage at being grouped as: 20% tin,
The nickel of 0.2-0.8%, the mischmetal of 0.1-1.0%, although the wetability of the solder is preferable, good mechanical performance.But pricker
The croop property of material is not pointed out, and soldered fitting is easy to generate creep under service condition.
Summary of the invention
Solder in the prior art there are the problem of have: constituent element is more, complicated, and practicability is very poor, at high cost.The present invention is directed to
Problems of the prior art, it is less to provide a kind of alloy constituent element, and it is convenient to smelt, and at low cost, easily controllable impurity lead contains
Amount, wettability is good, intensity with higher and suitable fusion temperature, specifically, creep-resistant property with higher.
The technical solution adopted by the present invention is that:
A kind of zinc-tin base leadless solder of high creep resistance, by following mass fraction at being grouped as:
19%~20% metallic tin；
0.1~2% metallic silver, or with 0.1~5 %CuP14 substitution；
Remaining ingredient is metallic zinc.
Further, the zinc-tin base leadless solder of high creep resistance is by following mass fraction at being grouped as:
19.92 the metallic tin of parts by weight；
The metallic silver of 1 parts by weight；
79.68 part by weight of metal zinc.
Further, the zinc-tin base leadless solder of high creep resistance is by following mass fraction at being grouped as:
19.98 the metallic tin of parts by weight；
The CuP14 of 0.1 parts by weight；
79.92 part by weight of metal zinc.
Further, the zinc-tin base leadless solder of high creep resistance is by following mass fraction at being grouped as:
19.92 the metallic tin of parts by weight；
The CuP14 of 0.5 parts by weight；
The metallic zinc of 79.6 parts by weight.
A kind of preparation method of the zinc-tin base leadless solder of high creep resistance, it the following steps are included:
(1) by weight by potassium chloride: lithium chloride=(1~1.6): the salt-mixture of (0.8~1.2) melts at 500 DEG C~550 DEG C
It is poured after change on the zinc and tin weighed up；
(2) load weighted Ag or CuP14 are added to molten by zinc, Xi Jiarewen to 700 DEG C~800 DEG C after zinc, tin fusing
In the molten metal melted, stirring；
(3) until completely melted, 1~2 hour is kept the temperature, stirring homogenizes alloy, and standing is come out of the stove, and surface is removed after solidification
Salt-mixture.
The present invention has the advantage that
The present invention has the advantages that can play the role of refining crystal grain with Dispersed precipitate in intrinsic silicon after Ag addition.P conduct
A kind of strong reducing property element.With preferable deoxidation effect.It can also be improved wetability after addition, refine crystal grain.And crystal grain
Refinement, can be improved the croop property of solder.Individually addition P has certain difficulty, present invention richness P in fusion process
CuPl4 alloy as intermediate alloy add.
The present invention has and fusion temperature similar in Zn20Sn lead-free brazing, suitable leadless soft soldering process conditions.This hair
Not only alloy constituent element is less for bright solder, practical, at low cost, nontoxic, pollution-free, and it is convenient to smelt, and soaks craftsmanship
Energy and shear strength are improved.Resistivity is not remarkably decreased, and creep-resistant property is preferable, suitable for the micro- of high-temperature field
Electronic Packaging.
Detailed description of the invention
Creep time-displacement curve of Fig. 1 solder.
Specific embodiment
Example 1: pouring after 26 grams of potassium chloride and 20 grams lithium chloride salt-mixtures are melted at 500 DEG C in 79.84 grams of zinc and
19.96 on gram tin.Furnace temperature is risen to 700 DEG C, 0.1 gram of Ag powder is added in solution after melting metal and salt-mixture, together
When be stirred continuously, formed alloy.Heat preservation 1 hour, is stirred continuously, homogenizes alloy.Standing is come out of the stove, and is removed after alloy graining
The salt-mixture on surface.
Example 2: pouring after 26 grams of potassium chloride and 20 grams lithium chloride salt-mixtures are melted at 520 DEG C in 79.68 grams of zinc and
19.92 on gram tin.Furnace temperature is risen to 750 DEG C, 1.0 grams of Ag powder are added in melt after melting metal and salt-mixture, together
When be stirred continuously, formed alloy；Heat preservation 1.5 hours, is stirred continuously, homogenizes alloy.Standing is come out of the stove, and is gone after alloy graining
Except the salt-mixture on surface.
Example 3: pouring after 23.4 grams of potassium chloride and 18 grams lithium chloride salt-mixtures are melted at 550 DEG C in 79.36 grams of zinc and
19.84 on gram tin.Furnace temperature is risen to 800 DEG C, 2.0 grams of Ag powder are added in melt after melting metal and salt-mixture, together
When be stirred continuously, formed alloy；Heat preservation 2 hours, is stirred continuously, homogenizes alloy.Standing is come out of the stove, and is removed after alloy graining
The salt-mixture on surface.
Example 4: pouring after 26 grams of potassium chloride and 20 grams lithium chloride salt-mixtures are melted at 500 DEG C in 79.92 grams of zinc and
19.98 on gram tin.Furnace temperature is risen to 710 DEG C, is added to 0.1 gram of CuP14 intermediate alloy after melting metal and salt-mixture molten
It in liquid, is stirred continuously simultaneously, forms alloy；Heat preservation 1 hour, is stirred continuously, homogenizes alloy.Standing is come out of the stove, to alloy
The salt-mixture on surface is removed after solidification.
Example 5: pouring after 32.5 grams of potassium chloride and 25 grams lithium chloride salt-mixtures are melted at 530 DEG C in 79.6 grams of zinc and
On 19.9 grams of tin.Furnace temperature is risen to 730 DEG C, 0.5 gram of CuP14 intermediate alloy is added to melt after melting metal and salt-mixture
In the middle, it is stirred continuously simultaneously, forms alloy；Heat preservation 1.5 hours, is stirred continuously, homogenizes alloy.Standing is come out of the stove, to alloy
The salt-mixture on surface is removed after solidification.
Example 6: it pours after 26 grams of potassium chloride and 20 grams lithium chloride salt-mixtures are melted at 550 DEG C in 79.2 grams of zinc and 19.8
On Ke Xi.Furnace temperature is risen to 800 DEG C, 5 grams of CuP14 intermediate alloys are added in melt after melting metal and salt-mixture,
It is stirred continuously simultaneously, forms alloy；Heat preservation 2 hours, is stirred continuously, homogenizes alloy.Standing is come out of the stove, and is gone after alloy graining
Except the salt-mixture on surface.
1 brazing filler metal alloy ingredient of table and fusion temperature
| Example | Zn g | Sn g | Ag g | CuP14 g | Fusion temperature (DEG C) |
| Comparative example | 80 | 20 | 0 | 0 | 383.43 |
| Embodiment 1 | 79.84 | 19.96 | 0.1 | 0 | 383.44 |
| Embodiment 2 | 79.68 | 19.92 | 1.0 | 0 | 383.55 |
| Embodiment 3 | 79.36 | 19.84 | 2.0 | 0 | 388.43 |
| Embodiment 4 | 79.92 | 19.98 | 0 | 0.1 | 383.30 |
| Embodiment 5 | 79.6 | 19.9 | 0 | 0.5 | 388.30 |
| Embodiment 6 | 79.2 | 19.8 | 0 | 5.0 | 378.37 |
Shear strength, spreading area and the resistivity of each brazing filler metal alloy of table 2
| Example | Shear strength (MPa) | Spreading area (mm2) | Resistivity (m Ω cm) |
| Comparative example | 19.7 | 43.2 | 0.0065 |
| Embodiment 1 | 25.0 | 40.3 | 0.0093 |
| Embodiment 2 | 23.2 | 50.7 | 0.0096 |
| Embodiment 3 | 23.3 | 47.3 | 0.0091 |
| Embodiment 4 | 30.0 | 47.7 | 0.007 |
| Embodiment 5 | 35.8 | 39.2 | 0.0075 |
| Embodiment 6 | 31.8 | 37.1 | 0.006 |
Claims (5)
1. a kind of zinc-tin base leadless solder of high creep resistance, which is characterized in that by following mass fraction at being grouped as:
19%~20% metallic tin；
0.1~2% metallic silver, or with 0.1~5 %CuP14 substitution；
Remaining ingredient is metallic zinc.
2. a kind of zinc-tin base leadless solder of high creep resistance as described in claim 1, which is characterized in that by following quality point
Number is at being grouped as:
19.92 the metallic tin of parts by weight；
The metallic silver of 1 parts by weight；
79.68 part by weight of metal zinc.
3. a kind of zinc-tin base leadless solder of high creep resistance as described in claim 1, which is characterized in that by following quality point
Number is at being grouped as:
19.98 the metallic tin of parts by weight；
The CuP14 of 0.1 parts by weight；
79.92 part by weight of metal zinc.
4. a kind of zinc-tin base leadless solder of high creep resistance as described in claim 1, which is characterized in that by following quality point
Number is at being grouped as:
19.92 the metallic tin of parts by weight；
The CuP14 of 0.5 parts by weight；
The metallic zinc of 79.6 parts by weight.
5. a kind of preparation method of the zinc-tin base leadless solder of high creep resistance, which is characterized in that it the following steps are included:
(1) by weight by potassium chloride: lithium chloride=(1~1.6): the salt-mixture of (0.8~1.2) melts at 500 DEG C~550 DEG C
It is poured after change on the zinc and tin weighed up；
(2) load weighted Ag or CuP14 are added to molten by zinc, Xi Jiarewen to 700 DEG C~800 DEG C after zinc, tin fusing
In the molten metal melted, stirring；
(3) until completely melted, 1~2 hour is kept the temperature, stirring homogenizes alloy, and standing is come out of the stove, and surface is removed after solidification
Salt-mixture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910244999.7A CN109894769B (en) | 2019-03-28 | 2019-03-28 | High-creep-resistance zinc-tin-based lead-free solder and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111571059A (en) * | 2020-05-29 | 2020-08-25 | 南昌大学 | Cerium-modified high-temperature zinc-tin-based alloy solder and preparation method and application thereof |
| 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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| US4112868A (en) * | 1976-05-24 | 1978-09-12 | Asahi Glass Company, Ltd. | Soldering apparatus |
| JPS55128396A (en) * | 1979-03-26 | 1980-10-04 | Packer Eng Ass | Zn alloy wax and its use |
| CN1215438A (en) * | 1996-02-23 | 1999-04-28 | 联合矿业有限公司 | Hot-dip galvanizing bath and process |
| US20070235503A1 (en) * | 2006-04-05 | 2007-10-11 | Mitsubishi Electric Corporation | Solder alloy and soldering method |
| 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 |
| CN106211763A (en) * | 2014-03-25 | 2016-12-07 | 住友金属矿山株式会社 | Coated solder material and manufacture method thereof |
| CN106536108A (en) * | 2014-04-17 | 2017-03-22 | 贺利氏材料新加坡私人有限公司 | Lead-free eutectic solder alloy comprising zinc as the main component and aluminum as an alloying metal |
| CN108115311A (en) * | 2017-12-18 | 2018-06-05 | 苏州铜宝锐新材料有限公司 | A kind of preparation method of low melting point brazing material |
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2019
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4112868A (en) * | 1976-05-24 | 1978-09-12 | Asahi Glass Company, Ltd. | Soldering apparatus |
| JPS55128396A (en) * | 1979-03-26 | 1980-10-04 | Packer Eng Ass | Zn alloy wax and its use |
| CN1215438A (en) * | 1996-02-23 | 1999-04-28 | 联合矿业有限公司 | Hot-dip galvanizing bath and process |
| US20070235503A1 (en) * | 2006-04-05 | 2007-10-11 | Mitsubishi Electric Corporation | Solder alloy and soldering method |
| CN106211763A (en) * | 2014-03-25 | 2016-12-07 | 住友金属矿山株式会社 | Coated solder material and manufacture method thereof |
| CN106536108A (en) * | 2014-04-17 | 2017-03-22 | 贺利氏材料新加坡私人有限公司 | Lead-free eutectic solder alloy comprising zinc as the main component and aluminum as an alloying 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 |
| CN108115311A (en) * | 2017-12-18 | 2018-06-05 | 苏州铜宝锐新材料有限公司 | A kind of preparation method of low melting point brazing material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111571059A (en) * | 2020-05-29 | 2020-08-25 | 南昌大学 | Cerium-modified high-temperature zinc-tin-based alloy solder and preparation method and application thereof |
| 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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| CN109894769B (en) | 2021-09-24 |
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