CN1301179C - Leadless solder - Google Patents
Leadless solder Download PDFInfo
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- CN1301179C CN1301179C CNB200510011704XA CN200510011704A CN1301179C CN 1301179 C CN1301179 C CN 1301179C CN B200510011704X A CNB200510011704X A CN B200510011704XA CN 200510011704 A CN200510011704 A CN 200510011704A CN 1301179 C CN1301179 C CN 1301179C
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- tin
- cerium
- lead
- silver
- copper
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Abstract
The present invention relates to a lead-free welding material, particularly to a lead-free welding material containing copper, silver and cerium. The present invention is characterized in that fine tin and metal cerium are cast into tin-cerium intermediate alloy ingots containing 4% of cerium after being smelted; the fine tin and silver ingots are cast into tin-silver intermediate alloy ingots containing 30 % of silver after being smelted; the fine tin and fine copper are cast into tin-copper intermediate alloy ingots containing 30 % of copper after being smelted; then, the three kinds of the intermediate alloy are added in a manganese alloy pot, and placed in an intermediate frequency furnace to be smelted and cast into a lead-free welding material rod, and the lead-free welding material of the present invention is obtained. The present invention has the advantages and the effects of high raw material purity, low metal loss in technological processes, uniform and refined metallic phases, good product quality and low price; the spread rate is enhanced, and the melting point is reduced; the shearing force of welding spots of chip components, the stretching force of the welding spots and the drawing force of QFP lead wires at 45 degrees are enhanced; thereby, the present invention belongs to an environmental protection product.
Description
Technical field
The present invention relates to a kind of lead-free welding material of a kind of lead-free solder, particularly cupric, silver and cerium, belong to the tin soldering alloys field.
The present invention relates to the manufacture method of this lead-free solder.
Background technology
Along with developing rapidly the requirement of electronic product of electronics industry is more and more higher, the used scolder kind of present electronic product is a lot, but majority still uses the tin-lead alloy scolder, because tin-kupper solder is leaded to have pollution to environment, therefore two instructions of European Union's issue, forbid electronic product, using leaded tin solder from July 1st, 2006, existing lead-free solder majority is Xi-Yin, tin-copper, tin-silver-copper, tin-zinc-indium-bismuth, tin-antimony-Yin-indium, tin-zinc-nickel etc. are formed, what also have minority is that Xi-Yin-mishmetal is formed, the weak point of above-mentioned lead-free welding material is the fusing point height that has, the wetability that has is little, the crystallization that has is thicker, the composition multiplex (MUX) who the has complicated cost height of planting.
Summary of the invention
Purpose of the present invention provides a kind of lead-free solder that fusing point is low, wetability good, cost is low that has for the shortcoming that overcomes above-mentioned prior art with deficiency just, thereby the welding material of high-quality is provided for the processing and manufacturing of electronic product.
The present invention also provides the manufacture method of this lead-free solder.
The objective of the invention is to be achieved through the following technical solutions:
A kind of lead-free solder is characterized in that what its employing following weight percentages was made:
Copper 0.3～3.0%, silver 0.5～6.0%, cerium 0.005～0.20%, surplus are tin,
Described raw material weight percentage is:
Copper 0.5～1.0%, cerium 0.01～0.1%, silver 3.0～3.5%, surplus are tin.
The manufacture method of lead-free solder is characterized in that it is undertaken by following step:
(a) be to add crucible at 96: 4 and insert vacuum melting furnace and carry out melting and be warming up to 1000 ℃ the refined tin of stanniferous 99.95% and the metallic cerium that contains cerium 99.99% by both weight ratio, be incubated 2 hours, stirred 30 minutes, and came out of the stove, cool off and cast the tin cerium intermediate alloy ingot that contains cerium 4%;
(b) be to add crucible at 70: 30 and insert the intermediate frequency furnace melting the silver ingot of the refined tin of stanniferous 99.95% and argentiferous 99.99% by both weight ratio, vacuum nitrogen filling gas, be warming up to 1200 ℃, be incubated 3 hours, come out of the stove, cool off the tin silver intermediate alloy ingot of casting argentiferous 30%;
(c) be to add crucible at 70: 30 and insert the intermediate frequency furnace melting the smart copper of the refined tin of stanniferous 99.95% and cupric 99.95% by both weight ratio, vacuum nitrogen filling gas, be warming up to 900 ℃, be incubated 3 hours, come out of the stove, cool off the tin copper intermediate alloy ingot of casting cupric 30%;
D) get tin cerium intermediate alloy ingot 0.125～5.0 weight portion of (a) item, (b) tin silver intermediate alloy ingot 1.67～20.0 weight portions and (c) Xiang Xitong intermediate alloy ingot 1.0～10.0 weight portions and not enough tin amount 77.42～90.0 weight portions of adding surplus tin, add in the manganese alloy pot simultaneously and insert the intermediate frequency furnace melting, vacuum nitrogen filling gas, be warming up to 450 ℃, come out of the stove, cool off and be cast into the lead-free solder rod, obtain containing the lead-free solder that copper, silver, cerium and surplus are tin.
The raw material that method of the present invention adopts is the tin slab of stanniferous 99.95%, the copper ingot of cupric 99.95%, the cerium ingot that contains cerium 99.99%, the silver ingot of argentiferous 99.95% is the market sale modular product, in the strict control of blending process, the cerium that adds in this product is a rare earth element, 789 ℃ of fusing points, 3426 ℃ of boiling points, density 6.77g/cm
3, it is the grey active metal, easily oxidation loses light and translates in air, heating flame is soluble in acid, is alloy material, but its deoxidation, desulfurization, evenly crystal grain thinning, improve mechanical performance and oxidation resistance, can reduce fusing point,
Product of the present invention detects through Ministry of Information Industry proprietary material quality supervision and test center, and its result is as follows:
1, solder joint stretching, shearing test, slice component solder joint shearing test, the QFP 45 ° of tension tests that go between, testing result sees Table 1
The stretching of table 1 solder joint, slice component solder joint shearing test, the QFP 45 ° of tension test testing results that go between
| Sample number into spectrum | Solder joint stretching (N) | Slice component solder joint shearing test (N) | The QFP 45 ° of tension tests (N) that go between | |||||
| 1# | Measured value | 204.2 | 197.8 | 30.3 | 23.1 | 24.9 | 26.2 | 21.4 |
| 240.5 | 209.3 | 27.9 | 28.5 | 21.4 | 23.6 | 21.7 | ||
| 240.9 | 26.8 | 23.5 | 25.3 | |||||
| Average | 218.5 | 27.3 | 23.5 | |||||
| 2# | Measured value | 230.8 | 233.8 | 29.6 | 37.0 | 21.5 | 24.1 | 20.8 |
| 194.4 | 227.9 | 27.6 | 20.3 | 28.3 | 23.7 | 25.6 | ||
| 213.4 | 32.8 | 27.4 | 20.3 | |||||
| Average | 220.1 | 31.5 | 22.7 | |||||
2, wetability
Testing result sees Table 2
Table 2 wetability testing result
| Sample number into spectrum | Wetting time started t 0(S) | Wetting rise time t 1(S) | Wetting time t (S) | Maximum wetting power F max(((mN))) ())) | Final wetting power F end(mN) | |
| 1# | 1 | 0.4 | 0.5 | 0.9 | 0.52 | 0.51 |
| 2 | 0.5 | 0.3 | 0.8 | 0.65 | 0.60 | |
| 3 | 0.6 | 0.3 | 0.9 | 0.74 | 0.49 | |
| 4 | 0.5 | 0.4 | 0.9 | 0.43 | 0.45 | |
| 5 | 0.4 | 0.4 | 0.8 | 0.67 | 0.50 | |
| Mean value | 0.5 | 0.4 | 0.9 | 0.60 | 0.51 | |
| 2# | 1 | 0.8 | 0.3 | 1.1 | 0.51 | 0.49 |
| 2 | 0.8 | 0.4 | 0.8 | 0.65 | 0.53 | |
| 3 | 0.6 | 0.5 | 1.1 | 0.61 | 0.59 | |
| 4 | 0.8 | 0.4 | 1.0 | 0.59 | 0.49 | |
| 5 | 0.6 | 0.3 | 0.9 | 0.65 | 0.62 | |
| Mean value | 0.7 | 0.4 | 1.0 | 0.60 | 0.54 | |
3, chemical composition detects
Testing result sees Table 3
Table 3 chemical composition testing result
| Test item | Sample number into spectrum | |
| 1# | 2# | |
| Sn(％) | 96.40 | 96.36 |
| Ag(％) | 2.97 | 2.98 |
| Cu(％) | 0.57 | 0.58 |
| Ce(％) | 0.010 | 0.076 |
| Pb(％) | 0.015 | 0.015 |
| Sb(％) | 0.013 | 0.011 |
| Fe(％) | 0.003 | 0.003 |
| Zn(％) | ＜0.0003 | ＜0.0003 |
| Bi(％) | 0.006 | 0.006 |
| AI(％) | ＜0.002 | ＜0.002 |
| As(％) | ＜0.003 | ＜0.003 |
| Cd(％) | ＜0.0005 | ＜0.0005 |
4, the rate of spread, fusing point, metallographic
Testing result sees Table 4
Table 4 rate of spread, fusing point, metallographic testing result
| Test item | Testing result | |
| 1# | 2# | |
| The rate of spread (%) | 78.0 | 77.6 |
| Fusing point (℃) | 219 | 219 |
| Metallographic | Metallographic structure is even | |
Conclusion: testing result shows that the sample metallographic structure is even, and performance indications are good, can be used as lead-free solder product new varieties.
5, performance relatively
Table 6 performance relatively
| Project | Import lead-free solder SnAGCu | Lead-free solder SnAgCuCe of the present invention |
| Elongation (%) | 78 | 78.4 |
| Wetability (mN) | 61 | 61 |
| Fusing point (℃) | 219 | 217 |
| Slice component solder joint shearing test (N) | 27.1 | 31.5 |
| Solder joint tension test (N) )(()) | 219.9 | 228.6 |
| The QFP 45 ° of tension tests (N) that go between | 23.3 | 23.5 |
| Metallographic (amplifying 200 times) | Crystallization is thicker | Crystallization is even |
Owing to take technique scheme to make the technology of the present invention compared with the prior art have following advantage and effect:
(a) the material purity height of this method employing, the technical process metal loss is low,
(b) lead-free solder of the present invention is owing to adopt cerium to make the rate of spread be raised to 78.4% by 78%, and fusing point is reduced to 217 ℃ by 219 ℃; Slice component solder joint shearing test is by 27.1
NBring up to 31.5
NThe solder joint tension test is high to 228.6N by 219.9/N, and 45 ° of tension tests of QFP lead-in wire are brought up to 23.5N by 23.3N, and metallographic is more even, more refinement,
(c) good product quality belongs to environment-friendly products, low price.
The specific embodiment
Embodiment 1
The refined tin 96kg of stanniferous 99.95% and the metallic cerium 4kg that contains cerium 99.99% are added crucible insert vacuum melting furnace and carry out melting, be warming up to 1000 ℃, be incubated 2 hours, stirred 30 minutes, come out of the stove, cool off and cast the tin cerium intermediate alloy ingot that contains cerium 4%; The refined tin 70kg of stanniferous 99.95% and the silver ingot 30kg adding crucible of argentiferous 99.99% are inserted the intermediate frequency furnace melting, and vacuum nitrogen filling gas is warming up to 1200 ℃, is incubated 3 hours, comes out of the stove, cools off the tin silver intermediate alloy ingot of casting argentiferous 30%; The refined tin 70kg of stanniferous 99.95% and the smart copper 30kg adding crucible of cupric 99.95% are inserted the intermediate frequency furnace melting, and vacuum nitrogen filling gas is warming up to 900 ℃, is incubated 3 hours, comes out of the stove, cools off the tin copper intermediate alloy ingot of casting cupric 30%; Get above-mentioned tin cerium intermediate alloy ingot 0.125kg, tin silver intermediate alloy ingot 20.0kg, tin copper intermediate alloy ingot 1.0kg and add the not enough tin amount 78.875kg of surplus tin, add manganese alloy melting pot and insert the intermediate frequency furnace melting, vacuum nitrogen filling gas, be warming up to 450 ℃, come out of the stove, cool off and be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.005%, silver 6.0%, copper 0.3%, tin 93.695% of the present invention.
Embodiment 2
Press the method for embodiment 1 and make three kinds of intermediate alloys, get tin-cerium alloy ingot 0.25kg, sn-ag alloy ingot 16.7kg, gun-metal ingot 1.67kg and add the not enough tin amount 81.38kg of surplus tin, add the fusing of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.01%, silver 5.0%, copper 0.5%, tin 94.49% of the present invention.
Embodiment 3
Press the method for embodiment 1 and make three kinds of intermediate alloys, get tin-cerium alloy ingot 1.25kg, sn-ag alloy ingot 13.33kg, gun-metal ingot 3.33kg and add the not enough tin amount 82.09kg of surplus tin, add the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.05%, silver 4.0%, copper 1.0%, tin 94.95% of the present invention.
Embodiment 4
Press the method for embodiment 1 and make three kinds of intermediate alloys, get tin-cerium alloy ingot 2.5kg, sn-ag alloy ingot 6.67kg, gun-metal ingot 6.67kg and add the not enough tin amount 84.16kg of surplus tin, add the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.1%, silver 2.0%, copper 2.0%, tin 95.9% of the present invention.
Embodiment 5
Press the method for embodiment 1 and make three kinds of intermediate alloys, the not enough tin amount 82.92kg that gets tin-cerium alloy ingot 3.75kg, sn-ag alloy ingot 3..33kg, gun-metal ingot 10kg and add surplus tin adds the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.15%, silver 1.00%, copper 3.0%, tin 95.85% of the present invention.
Embodiment 6
Press the method for embodiment 1 and make three kinds of intermediate alloys, the not enough tin amount 90kg that gets tin-cerium alloy ingot 5kg, sn-ag alloy ingot 1.67kg, gun-metal ingot 3.33kg and add surplus tin adds the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.2%, silver 0.5%, copper 1.0%, tin 98.3% of the present invention.
Embodiment 7
Press the method for embodiment 1 and make three kinds of intermediate alloys, the not enough tin amount 77.42kg that gets tin-cerium alloy ingot 0.25kg, sn-ag alloy ingot 20kg, gun-metal ingot 2.33kg and add surplus tin adds the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.01%, silver 6.0%, copper 0.7%, tin 93.29% of the present invention.
Embodiment 8
Press the method for embodiment 1 and make three kinds of intermediate alloys, get tin-cerium alloy ingot 2.5kg, sn-ag alloy ingot 10kg, gun-metal ingot 2.0kg and add the not enough tin amount 85.5kg of surplus tin, add the melting of manganese alloy melting pot, be cast into the lead-free solder rod, obtain the lead-free solder product of making for raw material by cerium 0.1%, silver 3.0%, copper 0.6%, tin 96.3% of the present invention.
Claims (3)
1, a kind of lead-free solder is characterized in that what its employing following weight percentages was made:
Copper 0.3～3.0%, silver 0.5～6.0%, cerium 0.005～0.20%, surplus are tin.
2, lead-free solder according to claim 1 is characterized in that described raw material weight percentage is:
Copper 0.5～1.0%, cerium 0.01～0.1%, silver 3.0～3.5%, surplus are tin.
3, the manufacture method of lead-free solder as claimed in claim 1 or 2 is characterized in that it is undertaken by following step:
(a) be to add crucible at 96: 4 and insert vacuum melting furnace and carry out melting and be warming up to 1000 ℃ the refined tin of stanniferous 99.95% and the metallic cerium that contains cerium 99.99% by both weight ratio, be incubated 2 hours, stirred 30 minutes, and came out of the stove, cool off and cast the tin cerium intermediate alloy ingot that contains cerium 4%;
(b) be to add crucible at 70: 30 and insert the intermediate frequency furnace melting the silver ingot of the refined tin of stanniferous 99.95% and argentiferous 99.99% by both weight ratio, vacuum nitrogen filling gas, be warming up to 1200 ℃, be incubated 3 hours, come out of the stove, cool off the tin silver intermediate alloy ingot of casting argentiferous 30%;
(c) be to add crucible at 70: 30 and insert the intermediate frequency furnace melting the smart copper of the refined tin of stanniferous 99.95% and cupric 99.95% by both weight ratio, vacuum nitrogen filling gas, be warming up to 900 ℃, be incubated 3 hours, come out of the stove, cool off the tin copper intermediate alloy ingot of casting cupric 30%;
(d) get 0.125～5.0 part of the tin cerium intermediate alloy ingot of (a), (b) 1.67～20.0 parts of tin silver intermediate alloy ingot and (c) 1.0～10.0 parts of Xiang Xitong intermediate alloy ingot and add 77.42～90.0 parts of the not enough tin amounts of surplus tin, add in the manganese alloy pot simultaneously and insert the intermediate frequency furnace melting, vacuum nitrogen filling gas, be warming up to 450 ℃, come out of the stove, cool off and be cast into the lead-free solder rod, obtaining containing copper, silver, cerium, surplus is the lead-free solder of tin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510011704XA CN1301179C (en) | 2005-05-11 | 2005-05-11 | Leadless solder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510011704XA CN1301179C (en) | 2005-05-11 | 2005-05-11 | Leadless solder |
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| Publication Number | Publication Date |
|---|---|
| CN1721124A CN1721124A (en) | 2006-01-18 |
| CN1301179C true CN1301179C (en) | 2007-02-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510011704XA Expired - Fee Related CN1301179C (en) | 2005-05-11 | 2005-05-11 | Leadless solder |
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| Country | Link |
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| CN (1) | CN1301179C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780607A (en) * | 2010-03-17 | 2010-07-21 | 华南理工大学 | Lead-free solder for electronic packaging, assembling and soldering and preparation method thereof |
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| CN105290640A (en) * | 2015-11-30 | 2016-02-03 | 苏州龙腾万里化工科技有限公司 | Lead-free soldering tin bar |
| CN109128569B (en) * | 2018-10-08 | 2021-12-07 | 广东中实金属有限公司 | Medium-low temperature lead-free solder and preparation method thereof |
| CN111347193A (en) * | 2020-04-16 | 2020-06-30 | 深圳市博士达焊锡制品有限公司 | High-reliability solder paste and preparation method thereof |
| CN114700651B (en) * | 2020-06-11 | 2024-04-05 | 中山翰华锡业有限公司 | Heat-resistant environment-friendly superfine soldering tin wire applied to intelligent manipulator welding and preparation method thereof |
| CN111590233B (en) * | 2020-06-11 | 2021-12-31 | 中山翰华锡业有限公司 | High-weldability environment-friendly superfine solder wire for intelligent manipulator welding and preparation method thereof |
| CN112779431B (en) * | 2020-12-25 | 2022-04-05 | 有研亿金新材料有限公司 | Method for improving sputtering property of palladium, silver and copper |
| CN114434040A (en) * | 2021-01-15 | 2022-05-06 | 重庆理工大学 | Dissimilar material interconnected zinc alloy mixed solder powder and connecting method |
| CN114289927A (en) * | 2021-12-28 | 2022-04-08 | 上海大学 | Lead-free solder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0270033A (en) * | 1988-03-31 | 1990-03-08 | Cookson Group Plc | Low toxity alloy composition for bonding and sealing |
| US5833921A (en) * | 1997-09-26 | 1998-11-10 | Ford Motor Company | Lead-free, low-temperature solder compositions |
| CN1398696A (en) * | 2002-09-06 | 2003-02-26 | 薛松柏 | Lead-free solder |
| US20040151616A1 (en) * | 2003-02-04 | 2004-08-05 | Sabarese Daniel M. | Lead-free alloys, composition thereof, methods of preparation and uses for soldering and babbitting |
| CN1554511A (en) * | 2003-12-26 | 2004-12-15 | 杨嘉骥 | Anti-oxidation lead-free solder and its preparing method |
-
2005
- 2005-05-11 CN CNB200510011704XA patent/CN1301179C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0270033A (en) * | 1988-03-31 | 1990-03-08 | Cookson Group Plc | Low toxity alloy composition for bonding and sealing |
| US5833921A (en) * | 1997-09-26 | 1998-11-10 | Ford Motor Company | Lead-free, low-temperature solder compositions |
| CN1398696A (en) * | 2002-09-06 | 2003-02-26 | 薛松柏 | Lead-free solder |
| US20040151616A1 (en) * | 2003-02-04 | 2004-08-05 | Sabarese Daniel M. | Lead-free alloys, composition thereof, methods of preparation and uses for soldering and babbitting |
| CN1554511A (en) * | 2003-12-26 | 2004-12-15 | 杨嘉骥 | Anti-oxidation lead-free solder and its preparing method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780607A (en) * | 2010-03-17 | 2010-07-21 | 华南理工大学 | Lead-free solder for electronic packaging, assembling and soldering and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1721124A (en) | 2006-01-18 |
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