CN104759783B - Low-silver lead-free solder and preparation method thereof - Google Patents
Low-silver lead-free solder and preparation method thereof Download PDFInfo
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- CN104759783B CN104759783B CN201510129531.5A CN201510129531A CN104759783B CN 104759783 B CN104759783 B CN 104759783B CN 201510129531 A CN201510129531 A CN 201510129531A CN 104759783 B CN104759783 B CN 104759783B
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- intermediate alloy
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a low-silver lead-free solder and a preparation method thereof. The low-silver lead-free solder consists of metal element components including, by weight, Ag 0.1%-1%, Cu 0.1%-1%, misch metal 0.01%-0.10% and the balance tin, wherein Ce accounts for 50%, La accounts for 25%, Nd accounts for 15% and Pr accounts for 10% in the misch metal. On the metal purity aspect, Ce >= 99.99%, La>= 99.99%, Nd >= 99.99%, Pr >= 99.99%, and Sn, Ag and Cu are industrial refined raw materials. The low-silver lead-free solder does not contain lead and can meet the lead-free welding requirement of electronic products. Branch-shaped primary-phase solid-liquid mixed slurry is crushed in an acute stirring mode in the low-silver hypo eutectic alloy solidification process, and a water-cooling casting forming mode is adopted to improve mechanical property, especially the plastic property. A rare earth alterant is adopted to achieve grain refinement, improve the wet performance of the solder and ensure long-term reliability of welding points.
Description
Technical field
The invention belongs to field of new, it is related to a kind of low-silver lead-free solder and preparation method thereof.
Background technology
Eutectic alloy sn96.5ag3cu0.5(sac305) use in a large number in electronics industry as tin-lead succedaneum, but
Ag amount height is contained, ag is noble metal, almost accounts for 1/2 in sac305 cost of alloy, cost greatly constrains electronic welding in solder
Lead-free and the development of technology.Hypoeutectic solder silver content is low, has optimal cost performance and receives significant attention, but hypoeutectic
Solder solid-liquid phase line interval larger (8 ~ 10 DEG C), alloy structure contains the nascent β sn phase of dendroid and sheet ag3Sn metal compound
Thing, causes solder wettability, mechanical property and welding spot reliability poor.
Patent No. cn102029479 a discloses a kind of lead-free solder alloy in low silver and preparation method thereof and device, adopts
The preparation method being combined with quick cooling and vibration, the method effectively reducing melting range and making alloy quick solidification, but this
Method is still limited to metal forming pattern under traditional single liquid condition, shakes merely with ultrasound wave in alloy graining process
Move it is difficult to reach the shearing strength needed for dendritic arm just ruptures from parent crystal, cause less efficient it is difficult to hypoeutectic is completely eliminated
The segregation tissue of dendrite in solder, has the risk of " rosin joint " and brittle failure as electronic solder.
Content of the invention
For eutectic alloy high cost, the deficiency of low silver alloy, the present invention provides a kind of low-silver lead-free solder and its preparation
Method, is obtained in that fine grain uniform formation, improves alloy mechanical property, improves solder wettability, improves welding spot reliability.
The present invention provide a kind of low-silver lead-free solder, described low-silver lead-free solder have following metallic element component and its
Percentage by weight:
Ag:0.1 ~ 1%, cu:0.1 ~ 1%, mischmetal: 0.01 ~ 0.10%, balance of stannum sn；
In mischmetal: ce:50%, la:25%, nd:15%, pr:10%；Each component metals purity: ce >=99.99%, la
>=99.99%, nd >=99.99%, pr >=99.99%；Sn, ag, cu are all using industrial refined material.
Preferably, the percentage by weight of described low-silver lead-free solder: ag:0.1 ~ 0.5%, cu:0.3 ~ 1%, mischmetal:
0.01 ~ 0.08%, balance of stannum sn.
The present invention also provides a kind of preparation method of described low-silver lead-free solder, has following steps:
(1) stannum and copper are added in graphite crucible, the weight of wherein copper accounts for the 5 ~ 15% of described alloy gross weight, be placed in true
Melting in empty induction melting furnace, temperature rises to 1100 ~ 1200 DEG C, and standing makes sn-cu intermediate alloy after its cooling；
(2) stannum and silver are added in graphite crucible, the weight of wherein silver accounts for the 5 ~ 10% of described alloy gross weight, be placed in true
Melting in empty induction melting furnace, temperature rises to 1000 ~ 1200 DEG C, and standing makes sn-ag intermediate alloy after its cooling；
(3) stannum and rare earth ce are added the amount adding rare earth ce in graphite crucible to account for the 1 ~ 3% of described weight alloy, be placed in
Melting in vacuum induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, and standing makes sn-ce intermediate alloy after its cooling；
(4) stannum and rare-earth la are added the amount adding rare-earth la in graphite crucible to account for the 1 ~ 3% of described weight alloy, be placed in
Melting in vacuum induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, and standing makes sn-la intermediate alloy after its cooling；
(5) stannum and rare earth pr are added the amount adding rare earth pr in graphite crucible to account for the 1% of described weight alloy, be placed in true
In empty induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, and standing makes sn-pr intermediate alloy after its cooling；
(6) stannum and rare earth nd are added the amount adding rare earth nd in graphite crucible to account for the 1% of described weight alloy, be placed in true
In empty induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, and standing makes sn- nd intermediate alloy after its cooling；
(7) by above-mentioned prepared intermediate alloy ingot and pure tin ag:0.1 ~ 1% by weight percentage, cu:0.1 ~ 1%, mixing is dilute
Soil 0.01 ~ 0.10%, wherein ce:50%, la:25%, nd:15%, pr:10%, balance of stannum；And add the kcl that mass ratio is 3:1
Form coverture with licl, be added in the equipment shown in Fig. 1 and carry out heating melting, after alloy molten, be cooled to 220 ~ 225 DEG C
When, incision mechanical agitation is simultaneously incubated 10 min, and supersonic vibration starts to apply until metal bath solidifies completely from liquid always,
Water-cooled.
Advantage of the present invention and beneficial effect:
(1) the low silver solder described in is not leaded, can meet the unleaded welding requirements of electronic product.
(2) using being stirred vigorously mode in the process of setting of low silver hypoeutectic alloy, the solid-liquid to dendroid primary phase
After mixed slurry carries out crushing, using the moulding by casting mode of water-cooled, the mechanical property particularly plasticity of solder can be improved.
(3) method with reference to rare earth alterative realizes crystal grain thinning, improve the wet performance of solder it is ensured that solder joint long-term
Reliability.
Brief description
Fig. 1 is the schematic diagram that the present invention prepares low-silver lead-free solder equipment.
Wherein: 1- adjustable speed agitator；2- heat insulating ability heating furnace；3- stainless steel crucible；4- temperature polling instrument (attached thermoelectricity
Even)；5- ultrasound wave sends out device；6- temperature control thermocouple.
Specific embodiment
, according to above-mentioned preparation method, the solder alloy composition of preparation and performance and its contrast are as shown in the table for the present invention.
From following table, and solder is cut churned mechanically temperature range and is narrowed with the increase of alloy containing silver amount, solid using half
Cut strong mechanical agitation under state, in conjunction with ultrasonic activation, dendrite knot group can be eliminated, the plasticity of solder is also improved；
The addition of rare earth affects less on tensile strength and elongation percentage, but appropriate mischmetal can improve the wettability of alloy well
Energy.
Claims (1)
1. a kind of preparation method of low-silver lead-free solder it is characterised in that: described low-silver lead-free solder has following metallic element
Component and its percentage by weight:
Ag:0.1 ~ 1%, cu:0.1 ~ 1%, mischmetal: 0.01 ~ 0.08%, balance of stannum sn；In mischmetal: ce:50%, la:
25%, nd:15%, pr:10%；Each component metals purity: ce >=99.99%, la >=99.99%, nd >=99.99%, pr >=
99.99%；Sn, ag, cu are all using industrial refined material；
The preparation method of this low-silver lead-free solder has following steps:
(1) stannum and copper are added in graphite crucible, be placed in melting in vacuum induction melting furnace, temperature rises to 1100 ~ 1200 DEG C, quiet
Put and make sn-cu intermediate alloy after its cooling, the weight of wherein copper accounts for the 5 ~ 15% of described intermediate alloy gross weight；
(2) stannum and silver are added in graphite crucible, be placed in melting in vacuum induction melting furnace, temperature rises to 1000 ~ 1200 DEG C, quiet
Put and make sn-ag intermediate alloy after its cooling, the weight of wherein silver accounts for the 5 ~ 10% of described intermediate alloy gross weight；
(3) stannum and rare earth ce are added in graphite crucible, be placed in melting in vacuum induction melting furnace, temperature rises to 1100 ~ 1300
DEG C, standing makes sn-ce intermediate alloy after its cooling, and the amount of its middle rare earth ce accounts for the 1 ~ 3% of described intermediate alloy weight；
(4) stannum and rare-earth la are added in graphite crucible, be placed in melting in vacuum induction melting furnace, temperature rises to 1100 ~ 1300
DEG C, standing makes sn-la intermediate alloy after its cooling, and the amount of wherein rare-earth la accounts for the 1 ~ 3% of described intermediate alloy weight；
(5) stannum and rare earth pr are added in graphite crucible, be placed in vacuum induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, quiet
Put and make sn-pr intermediate alloy after its cooling, the amount of its middle rare earth pr accounts for the 1% of described intermediate alloy weight；
(6) stannum and rare earth nd are added in graphite crucible, be placed in vacuum induction melting furnace, temperature rises to 1100 ~ 1300 DEG C, quiet
Put and make sn- nd intermediate alloy after its cooling, the amount of its middle rare earth nd accounts for the 1% of described intermediate alloy weight；
(7) by above-mentioned prepared intermediate alloy ingot and pure tin ag:0.1 ~ 1% by weight percentage, cu:0.1 ~ 1%, mischmetal
0.01 ~ 0.08%, ce:50%, la:25%, nd:15%, pr:10% in mischmetal, balance of stannum configuration；And add the mass ratio to be
Kcl the and licl composition coverture of 3:1, carries out in addition equipment heating melting, when being cooled to 220 ~ 225 DEG C after alloy molten,
Incision mechanical agitation is simultaneously incubated 10 min, and supersonic vibration starts to apply until metal bath solidifies completely from liquid always, water
Cold.
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| CN201510129531.5A CN104759783B (en) | 2015-03-24 | 2015-03-24 | Low-silver lead-free solder and preparation method thereof |
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| CN201510129531.5A CN104759783B (en) | 2015-03-24 | 2015-03-24 | Low-silver lead-free solder and preparation method thereof |
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| CN104759783A CN104759783A (en) | 2015-07-08 |
| CN104759783B true CN104759783B (en) | 2017-02-01 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106181110B (en) * | 2016-08-16 | 2018-11-23 | 镇江市锶达合金材料有限公司 | A kind of preparation method of rare earth alloy solder |
| CN106312360A (en) * | 2016-09-28 | 2017-01-11 | 深圳市唯特偶新材料股份有限公司 | Low-temperature welding material and preparation method thereof |
| CN107447128A (en) * | 2017-07-10 | 2017-12-08 | 西安理工大学 | A kind of low-melting alloy and preparation method thereof |
| CN107825003B (en) * | 2017-12-12 | 2020-01-10 | 云南锡业锡材有限公司 | Preparation method of soldering flux for soldering paste and ultrasonic rapid cooling system thereof |
| 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 |
| 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 |
| CN114952072B (en) * | 2021-12-26 | 2024-04-12 | 昆明理工大学 | Six-element Sn-Bi lead-free solder and preparation method thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4391276B2 (en) * | 2004-03-12 | 2009-12-24 | 新日鉄マテリアルズ株式会社 | Solder alloy for semiconductor mounting, manufacturing method thereof, solder ball, electronic member |
| JP2009506203A (en) * | 2005-08-24 | 2009-02-12 | フライズ メタルズ インコーポレイテッド | Solder alloy |
| CN101700606B (en) * | 2009-11-27 | 2011-11-30 | 浙江一远电子科技有限公司 | Sn-Ag-Cu misch metal lead-free solder with low content of Cu and preparation method thereof |
| CN102294553B (en) * | 2011-07-21 | 2013-10-16 | 北京工业大学 | Magnesium alloy brazing filler metal containing rare-earth element Er and preparation method thereof |
| CN102615447B (en) * | 2012-03-26 | 2014-11-05 | 广东工业大学 | Tin-based lead-free solder and preparation method thereof |
| CN102896436B (en) * | 2012-10-10 | 2014-10-29 | 常熟市华银焊料有限公司 | Sn-Ag-Cu lead-free solder containing Nd, Se and Ga |
| CN103056543B (en) * | 2013-01-18 | 2015-03-25 | 江苏师范大学 | Lead-free nanometer solder containing Yb, A1 and B |
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Application publication date: 20150708 Assignee: Gaoxin Tin Industry (Huizhou) Co., Ltd. Assignor: Guangdong University of Technology Contract record no.: 2018440000010 Denomination of invention: Low-silver lead-free solder and preparation method thereof Granted publication date: 20170201 License type: Common License Record date: 20180207 |
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