CN1292316A - Rare earth contained tin base lead-less solder and its preparation method - Google Patents
Rare earth contained tin base lead-less solder and its preparation method Download PDFInfo
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- CN1292316A CN1292316A CN 00129872 CN00129872A CN1292316A CN 1292316 A CN1292316 A CN 1292316A CN 00129872 CN00129872 CN 00129872 CN 00129872 A CN00129872 A CN 00129872A CN 1292316 A CN1292316 A CN 1292316A
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- Prior art keywords
- tin
- rare earth
- flux
- mixing salt
- repone
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 31
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910000679 solder Inorganic materials 0.000 title abstract description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 34
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 27
- 239000000956 alloy Substances 0.000 claims abstract description 27
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 241001062472 Stokellia anisodon Species 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 12
- 229910052702 rhenium Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 abstract description 56
- 238000005219 brazing Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 7
- 229910052797 bismuth Inorganic materials 0.000 abstract description 6
- 238000005476 soldering Methods 0.000 abstract description 3
- 229910001128 Sn alloy Inorganic materials 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The composition of said invented brazing alloy contains (wt%) 1-7% of Ag, 2-8% of Bi, 1-30% of Sn-Re, and the rest is Sn, in which the above-mentioned Sn-Re contains 1-10% of Re. Its preparation method includes the following steps: under the condition of protection of potassium chloride and lithium chloride mixed salt pressing rare earth into tin liquor to smelt intermediate alloy of tin, then adding said intermediate alloy, Ag and Bi into the molten tin liquor, after solidification removing mixed salt from surface. As compared with traditional solder the wettability of said invented solder containing rare earth is superior to traditional solder, and its mechanical properties are raised, so that it is applicable to soft soldering in electronic industry.
Description
A kind of tin base leadless soldering-flux that contains rare earth and preparation method thereof belongs to tin base leadless soldering-flux manufacturing technology field.
In order to adapt to the unleaded trend in the whole world, many countries have taken up to research and produce lead-free product, and have developed the lead-free alloy of multiple composition.For example, United States Patent (USP) 4,929,423 Sn-(0.08-20%) Bi-(0.01-1.5%) Ag-(0.02-1.5%) the Cu-0.01%P-mishmetals that propose, still, this alloy series is mainly used in the pipeline soldering, it is hexa-atomic alloy, make difficulty, not protection in the solder smelting process, the alloying element scaling loss is serious; The molten temperature region of this solder big (～28 ℃) is not suitable for using in electron trade.In addition, also has United States Patent (USP) 499, Sn-(3.1-7%) Ag-(6-30%) Bi that Sn-(3-5%) Ag-(1.2-3%) Bi that 452 Sn-(0.1-3%) Ag-(3-7%) Bi that propose, Japanese flat 5-228685 propose and Chinese patent CN1139609 propose, the molten temperature region of the various compositions of this alloy series is roughly at 185-215 ℃, and its reflow welding temperature also can be controlled in the 230-240 ℃ of scope.But, these alloy series or not protection, the alloying element scaling loss is serious; Or under vacuum or rare gas element, smelt, the temperature height, the time is long, complex process, the wettability of solder is bad simultaneously, brings weldability relatively poor; Simultaneously, the needle-like that runs through matrix and thick intermetallic compound Ag in irregular shape have been produced in these tin base leadless soldering-flux (SnAgBi) inside that do not contain rare earth
3Sn makes that the plasticity of solder is poor, and obdurability reduces, and then has reduced fatigue lifetime.
The objective of the invention is to overcome problems of the prior art, what a kind of wettability, good mechanical properties were provided contains tin base leadless soldering-flux of rare earth and preparation method thereof
The tin base leadless soldering-flux that contains rare earth provided by the invention is characterized in that: contain the Ag that weight ratio is 1-7%, the Bi of 2-8%, 1～30% master alloy Sn-Re, all the other are Sn, wherein, contain weight ratio among the described master alloy Sn-Re and be 1～10% Re, Re is a mishmetal.
The preparation method who contains the tin base leadless soldering-flux of rare earth provided by the invention, it is characterized in that: it may further comprise the steps: (1) is smelt mishmetal the master alloy Sn-Re of tin: with Repone K: water after the mixing salt heat fused of lithium chloride=1.3: 1 (weight ratio) and make the tin fusing on tin, and be heated to 500～900 ℃, mishmetal is pressed into also continuous stirring of tin liquor to be melted fully until rare earth, insulation, come out of the stove after leaving standstill, solidify the mixing salt that the surface is removed in the back; (2) with Repone K: water on tin after the mixing salt heat fused of lithium chloride=1.3: 1 (weight ratio), master alloy Sn-Re and Ag, the Bi of tin are added in the fused tin liquor, constantly stir simultaneously, insulation, come out of the stove after leaving standstill, solidify the mixing salt that the surface is removed in the back.
Because rare earth is very easily oxidized, if directly in atmosphere, be added to rare earth in the solder alloy, scaling loss is very serious, simultaneously, the scaling loss of Bi element in atmosphere is also very serious, therefore, adopts in the present invention: (1) is under the mixing salt protection, Sn and Re are smelt master alloy Sn-Re, and the rare earth that adequately protects is not by scaling loss; (2) under the mixing salt protection, master alloy Sn-Re, Ag, Bi are added in the tin liquor, reduce the scaling loss of alloying element and rare earth.
Description of drawings: Fig. 1: the comparison of the tin base leadless soldering-flux of example 1 of the present invention and example 2 and traditional tin base leadless soldering-flux spreading area; Fig. 2: the comparison of the tin base leadless soldering-flux of example 1 of the present invention and example 2 and traditional tin base leadless soldering-flux mechanical property; Fig. 3: traditional tin base leadless soldering-flux micro-organization chart; Fig. 4: the tin base leadless soldering-flux micro-organization chart of example 1 of the present invention.
Embodiment:
Example 1, take by weighing 130 gram Repone K, 100 grams lithium chlorides and put into alumina crucible, mix back heat fused to 600 ℃ in resistance furnace, fused salt poured on 96.52% the tin and make the tin fusing, and in intermediate frequency furnace, be heated to 600 ℃, then, with the foraminate graphite bell jar of peripheral band 3.48% mishmetal (commercially available) is pressed into tin liquor and constantly stirs and melt fully until rare earth, be incubated 30 minutes, leave standstill after 10 minutes and come out of the stove, remove the Repone K and the lithium chloride mixing salt on surface, the alloy liquation is cast into lamellar so that take by weighing.Water on 86.82% tin after the mixing salt heat fused with 130 gram Repone K, 100 grams lithium chlorides, Sn-Re master alloy with 7.18% and 1% Ag, 5% Bi join in the fused tin liquor, constantly stir simultaneously, be incubated 30 minutes, leave standstill the cooling of coming out of the stove after 10 minutes, solidify Repone K and lithium chloride mixing salt that the surface is removed in the back.The solder piece reheated be melted to 350 ℃, the pricker liquid of molten state is watered on angle steel slightly with angle, it is stand-by to make it be cooled to strip fast.
Example 2, take by weighing 130 gram Repone K, 100 grams lithium chlorides and put into alumina crucible, mix back heat fused to 600 ℃ in resistance furnace, fused salt poured on 96.52% the tin and make the tin fusing, and in intermediate frequency furnace, be heated to 600 ℃, then, with the foraminate graphite bell jar of peripheral band 3.48% mishmetal (commercially available) is pressed into tin liquor and constantly stirs and melt fully until rare earth, be incubated 30 minutes, leave standstill after 10 minutes and come out of the stove, remove the Repone K and the lithium chloride mixing salt on surface, the alloy liquation is cast into lamellar so that take by weighing.Water on 84.88% tin after the mixing salt heat fused with 130 gram Repone K, 100 grams lithium chlorides, Sn-Re master alloy with 8.62% and 3.5% Ag, 3% Bi join in the fused tin liquor, constantly stir simultaneously, be incubated 30 minutes, leave standstill the cooling of coming out of the stove after 10 minutes, solidify Repone K and lithium chloride mixing salt that the surface is removed in the back.The solder piece reheated be melted to 350 ℃, the pricker liquid of molten state is watered on angle steel slightly with angle, it is stand-by to make it be cooled to strip fast.
Example 3, take by weighing 130 gram Repone K, 100 grams lithium chlorides and put into alumina crucible, mix back heat fused to 600 ℃ in resistance furnace, fused salt poured on 96.52% the tin and make the tin fusing, and in intermediate frequency furnace, be heated to 600 ℃, then, with the foraminate graphite bell jar of peripheral band 3.48% mishmetal (commercially available) is pressed into tin liquor and constantly stirs and melt fully until rare earth, be incubated 30 minutes, leave standstill after 10 minutes and come out of the stove, remove the Repone K and the lithium chloride mixing salt on surface, the alloy liquation is cast into lamellar so that take by weighing.Water on 74.63% tin after the mixing salt heat fused with 130 gram Repone K, 100 grams lithium chlorides, Sn-Re master alloy with 14.37% and 5% Ag, 6% Bi join in the fused tin liquor, constantly stir simultaneously, be incubated 30 minutes, leave standstill the cooling of coming out of the stove after 10 minutes, solidify Repone K and lithium chloride mixing salt that the surface is removed in the back.The solder piece reheated be melted to 350 ℃, the pricker liquid of molten state is watered on angle steel slightly with angle, it is stand-by to make it be cooled to strip fast.
Example 4, take by weighing 130 gram Repone K, 100 grams lithium chlorides and put into alumina crucible, mix back heat fused to 600 ℃ in resistance furnace, fused salt poured on 96.52% the tin and make the tin fusing, and in intermediate frequency furnace, be heated to 600 ℃, then, with the foraminate graphite bell jar of peripheral band 3.48% mishmetal (commercially available) is pressed into tin liquor and constantly stirs and melt fully until rare earth, be incubated 30 minutes, leave standstill after 10 minutes and come out of the stove, remove the Repone K and the lithium chloride mixing salt on surface, the alloy liquation is cast into lamellar so that take by weighing.Water on 82.63% tin after the mixing salt heat fused with 130 gram Repone K, 100 grams lithium chlorides, Sn-Re master alloy with 2.87% and 7% Ag, 7.5% Bi join in the fused tin liquor, constantly stir simultaneously, be incubated 30 minutes, leave standstill the cooling of coming out of the stove after 10 minutes, solidify Repone K and lithium chloride mixing salt that the surface is removed in the back.The solder piece reheated be melted to 350 ℃, the pricker liquid of molten state is watered on angle steel slightly with angle, it is stand-by to make it be cooled to strip fast.
Below by some charts and example performance after solder of the present invention improves is described.For ease of comparing, the present invention contains the tin base leadless soldering-flux of rare earth and traditional tin base leadless soldering-flux all obtains under aforementioned the same terms.
In the table 1, example 1-4 is the lead-free brazing that contains rare earth, and example 5,6 is traditional tin base leadless soldering-flux that does not contain rare earth.Solidus temperature and liquidus temperature record with differential thermal analysis.It can also be seen that from table 1 example 1-4 has the temperature of fusion scope close with traditional tin base leadless soldering-flux, be fit to the electron trade soldering and use.
Fig. 1 has represented the comparison of the lead-free brazing spreading area that contains rare earth of traditional tin base leadless soldering-flux and the present invention development, and wherein, 1 and 2 is that example 1 and example 2,6 are example 6 in the table 1 in the table 1.By among Fig. 1 as can be seen, the spreading area of example 1 of the present invention and example 2 is greater than traditional tin base leadless soldering-flux, illustrates that its wettability improves.
Fig. 2 be the tensile strength of the lead-free brazing that contains rare earth developed of the present invention and traditional tin base leadless soldering-flux and unit elongation relatively, wherein, 1 and 2 is that example 1 and example 2,6 are example 6 in the table 1 in the table 1.As can be seen from Figure 2, compare with traditional tin base leadless soldering-flux, the tensile strength and the unit elongation of example 1 of the present invention and example 2 all are better than the former, show that its obdurability is improved.
For from the microcosmic angle analysis with the performance of this alloy is described, can be able to further confirmation by observing microstructure.Now the microstructure of the lead-free brazing that contains rare earth that traditional tin base leadless soldering-flux and the present invention are developed compares.See shown in Fig. 3,4.
Among Fig. 3 (magnification is 400), compd A g between bulk in irregular shape and needle-like metal is distributing in traditional tin base leadless soldering-flux
3Sn is because intermetallic compound Ag
3Sn is fragility and exists mutually, acicular Ag
3Sn plays a part to isolate matrix, serves as formation of crack; The present invention contain add an amount of rare earth in the lead-free brazing of rare earth after, by Fig. 4 (magnification is 400) as can be seen, Ag
3Sn is even, tiny spot distribution, thereby plays the effect of highly malleablized.
In sum; because the present invention has added proper amount of rare-earth, and adopts the salt flux guard method in the whole process of preparation, smelt its wettability of the tin base leadless soldering-flux that contains rare earth that thus and be better than traditional lead-free brazing; tissue is significantly improved, and mechanical property is improved.
Table 1
| Example | ????1 | ????2 | ?3 | ????4 | ????5 | ????6 |
| ?Sn(％) | ????86.82 | ????84.88 | ?74.63 | ????82.63 | ????91.84 | ????91.7 |
| ?Ag(％) | ????1 | ????3.5 | ?5 | ????7 | ????3.33 | ????3.5 |
| ?Bi(％) | ????5 | ????3 | ?6 | ????7.5 | ????4.83 | ????4.8 |
| ?Sn-Re(％) | ????7.18 | ????8.62 | ?14.37 | ????2.87 | ????-- | ????-- |
| Solidus temperature (℃) | ????198 | ????206 | ?209 | ????210 | ????205 | ????206 |
| Liquidus temperature (℃) | ????205 | ????213 | ?215 | ????216 | ????210 | ????211 |
| The temperature of fusion scope (℃) | ????7 | ????7 | ?6 | ????6 | ????5 | ????5 |
Claims (2)
1, a kind of tin base leadless soldering-flux that contains rare earth is characterized in that: contain the Ag that weight ratio is 1-7%, the Bi of 2-8%, 1～30% master alloy Sn-Re, all the other are Sn, wherein, contain weight ratio among the described master alloy Sn-Re and be 1～10% Re, Re is a mishmetal.
2, a kind of preparation method who contains the tin base leadless soldering-flux of rare earth, it is characterized in that: it may further comprise the steps: (1) is smelt mishmetal the master alloy Sn-Re of tin: with Repone K: water after the mixing salt heat fused of lithium chloride=1.3: 1 (weight ratio) and make the tin fusing on tin, and be heated to 500～900 ℃, mishmetal is pressed into also continuous stirring of tin liquor to be melted fully until rare earth, insulation, come out of the stove after leaving standstill, solidify the mixing salt that the surface is removed in the back; (2) with Repone K: water on tin after the mixing salt heat fused of lithium chloride=1.3: 1 (weight ratio), master alloy Sn-Re and Ag, the Bi of tin are added in the fused tin liquor, constantly stir simultaneously, insulation, come out of the stove after leaving standstill, solidify the mixing salt that the surface is removed in the back.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00129872 CN1128037C (en) | 2000-10-24 | 2000-10-24 | Rare earth contained tin base lead-less solder and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00129872 CN1128037C (en) | 2000-10-24 | 2000-10-24 | Rare earth contained tin base lead-less solder and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1292316A true CN1292316A (en) | 2001-04-25 |
| CN1128037C CN1128037C (en) | 2003-11-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00129872 Expired - Fee Related CN1128037C (en) | 2000-10-24 | 2000-10-24 | Rare earth contained tin base lead-less solder and its preparation method |
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| Country | Link |
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| CN (1) | CN1128037C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ300575B6 (en) * | 2005-01-04 | 2009-06-17 | Jeník@Jan | Lead-free solder |
| CN102248318A (en) * | 2011-06-30 | 2011-11-23 | 哈尔滨工业大学 | Low-silver and oxidation-resistant Sn-Ag system lead-free solder |
| CN101381826B (en) * | 2008-09-26 | 2012-11-07 | 南昌大学 | Sn-Cu base leadless solder alloy and preparation method |
| CN107177751A (en) * | 2017-04-25 | 2017-09-19 | 广西大学 | Good lead-free solder of a kind of corrosion-resistant and wetability and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100352596C (en) * | 2005-07-22 | 2007-12-05 | 沈阳工业大学 | Lead-free soft brazing alloy containing mixed rare earth and production thereof |
-
2000
- 2000-10-24 CN CN 00129872 patent/CN1128037C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ300575B6 (en) * | 2005-01-04 | 2009-06-17 | Jeník@Jan | Lead-free solder |
| CN101381826B (en) * | 2008-09-26 | 2012-11-07 | 南昌大学 | Sn-Cu base leadless solder alloy and preparation method |
| CN102248318A (en) * | 2011-06-30 | 2011-11-23 | 哈尔滨工业大学 | Low-silver and oxidation-resistant Sn-Ag system lead-free solder |
| CN102248318B (en) * | 2011-06-30 | 2012-12-05 | 杭州华光焊接新材料股份有限公司 | Low-silver and oxidation-resistant Sn-Ag system lead-free solder |
| CN107177751A (en) * | 2017-04-25 | 2017-09-19 | 广西大学 | Good lead-free solder of a kind of corrosion-resistant and wetability and preparation method thereof |
| CN107177751B (en) * | 2017-04-25 | 2019-08-30 | 广西大学 | The good lead-free solder and preparation method thereof of a kind of corrosion-resistant and wetability |
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| Publication number | Publication date |
|---|---|
| CN1128037C (en) | 2003-11-19 |
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