CN1337293A - Rare earth-containing tin-base lead-less brazing alloy and its prepn - Google Patents
Rare earth-containing tin-base lead-less brazing alloy and its prepn Download PDFInfo
- Publication number
- CN1337293A CN1337293A CN 01131275 CN01131275A CN1337293A CN 1337293 A CN1337293 A CN 1337293A CN 01131275 CN01131275 CN 01131275 CN 01131275 A CN01131275 A CN 01131275A CN 1337293 A CN1337293 A CN 1337293A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- tin
- flux
- leadless soldering
- base leadless
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 35
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 35
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 16
- 239000000956 alloy Substances 0.000 title claims abstract description 16
- 238000005219 brazing Methods 0.000 title description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 54
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 11
- 239000001103 potassium chloride Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 229910020994 Sn-Zn Inorganic materials 0.000 claims abstract description 8
- 229910009069 Sn—Zn Inorganic materials 0.000 claims abstract description 8
- 239000011833 salt mixture Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052702 rhenium Inorganic materials 0.000 claims description 9
- 230000004927 fusion Effects 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 2
- 229910000679 solder Inorganic materials 0.000 abstract description 25
- 150000003839 salts Chemical class 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000011701 zinc Substances 0.000 abstract 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 description 22
- 238000005260 corrosion Methods 0.000 description 22
- 229910005728 SnZn Inorganic materials 0.000 description 12
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 230000010287 polarization Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- 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
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002161 passivation Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241001269238 Data Species 0.000 description 1
- 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 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The present invention relates to a tin base lead-free solder containing rare earth and its preparation method. It contains 4-10 % of Zn, 0.05-1% of Re, and the rest is Sn. Its preparation method includes the following steps: heating mixed salt formed from potassium chloride and lithium chloride according to the weight ratio of 1.3:1 to 500-600 deg.C to make them melt; pouring the above-mentioned melted material on the tin, after the tin is completely metal, adding zinc 5o molten tin to make Zn melt, then quickly pressing rare earth into the molten mixed salt and Sn-Zn alloy, heat-insulating at 400-500 deg.C, standing still, after the above-mentioned material is coagulated, removing surface mixed salt. The invented solder possesses excellent anti-corrosive property, and can be extensively used in the electronic industry.
Description
One, technical field
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.
Two, background technology
Connection needs good corrosion resistance with lead-free brazing as novel electron.Traditional SnZn brazing filler metal alloy corrosion resistance is relatively poor.For solving its corrosion resistance problem, United States Patent (USP) 5,242,658 (72.28-89.4) Sn-(6.7-19.2) Zn-(2.7-19.4) In that propose, by adding In at traditional Sn-Zn alloy, the oxidation and the against corrosion and waste residue that have solved Zn form problem.But, owing to add the result of In, in microstructure, having formed irregular needle-like dendrite, thereby reduced mechanical strength, the result has weakened final bond strength.Simultaneously, In is low at earth's crust content, the price height, and its adding must bring the rising significantly of solder cost.On the solder preparation method, Chinese patent CN 1292316A discloses a kind of preparation method who contains the tin base leadless soldering-flux of rare earth, it is characterized in that adopting two step smelting methods, the first step is with after Sn refines into intermediate alloy with rare earth, second step joined the intermediate alloy of rare earth and Sn in the final molten alloy again, and whole preparation section is more numerous and diverse.
Three, summary of the invention
The present invention is directed to problems of the prior art, provide the good and technology of a kind of corrosion resistance simply to contain 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 percentage by weight and be 4～10% Zn, and 0.05～1% Re, all the other are Sn, wherein, Re is a mishmetal.
The above-described tin base leadless soldering-flux that contains rare earth is characterized in that: it is 5～10% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.1～1% Re, and all the other are Sn.
The above-described tin base leadless soldering-flux that contains rare earth is characterized in that: it is 6～9% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.05～0.6% Re, and all the other are Sn.
The above-described tin base leadless soldering-flux that contains rare earth is characterized in that: it is 8～9% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.1～0.2% Re, and all the other are Sn.
The preparation method who contains the tin base leadless soldering-flux of rare earth provided by the invention, it is characterized in that: (1) is with potassium chloride: the salt-mixture of lithium chloride=1.3: 1 (weight ratio) is watering after 500～600 ℃ of heat fused on the tin that is weighing up, after treating that tin melts fully, Zn is joined in the tin liquor of fusion, stir, make the Zn fusing; (2) rare earth is pressed into rapidly in the salt-mixture and Sn-Zn alloy of fusion, stirs, rare earth is melted fully; (3) 400～500 ℃ of insulations, treat that alloy mixes after, the salt-mixture that the surface is removed in the back is solidified in the cooling of coming out of the stove after leaving standstill.
Because rare earth is very easily oxidized, if directly rare earth is joined in atmosphere in the brazing filler metal alloy, scaling loss is very serious; the Zn element also is easy to oxidized, therefore, adopts in the present invention under the salt-mixture protection; Zn, Re are joined in the tin liquor successively, reduce the scaling loss of alloying element and rare earth.
The amount that adds rare earth in the alloy of the present invention should be limited in 0.05-1%.The adding of rare earth can make brazing seam structure's refinement, even, and barrier potential sclerosis and multiple slip induration increase, and helps to reduce its corrosion equilibrium potential, thereby improves its resistance to corrosion.
Four, description of drawings
Fig. 1: the comparison of the corrosion equilibrium potential of the tin base leadless soldering-flux of example 3 of the present invention and example 4 and traditional tin base leadless soldering-flux;
Fig. 2: the comparison of the corrosion rate of the tin base leadless soldering-flux of example 3 of the present invention and example 4 and traditional tin base leadless soldering-flux;
Fig. 3: traditional tin base leadless soldering-flux SnZn anodic polarization curves;
Fig. 4: traditional tin base leadless soldering-flux SnZnAgBi anodic polarization curves;
Fig. 5: the tin base leadless soldering-flux anodic polarization curves of example 4 of the present invention.
Five, the specific embodiment
Example 1: take by weighing 130 gram potassium chloride, 100 grams lithium chlorides and put into alumina crucible, mix, Heat fused to 600 ℃, the pure tin that fused salt is watered 95.5% melts tin fully, under 450 ℃, Zn with 4% joins in the tin liquor of melting, constantly stirs simultaneously, makes the Zn fusing; 0.5% rare earth is fast Ram compression enters in the salt-mixture and Sn-Zn alloy of melting, stirs fusing; Be incubated 30 minutes, left standstill 10 fens Rear potassium chloride and the lithium chloride salt-mixture of removing the surface solidified in the cooling of coming out of the stove behind the clock. The solder piece is added again Heat fusing to 350 ℃ waters the pricker liquid of molten state on angle steel slightly with angle, makes its fast cooling slivering Shape is stand-by.
Example 2: take by weighing 130 gram potassium chloride, 100 grams lithium chlorides and put into alumina crucible, mix, Heat fused to 600 ℃, the pure tin that fused salt is watered 93.8% melts tin fully, under 450 ℃, Zn with 6% joins in the tin liquor of melting, constantly stirs simultaneously, makes the Zn fusing; 0.2% rare earth is fast Ram compression enters in the salt-mixture and Sn-Zn alloy of melting, stirs fusing; Be incubated 30 minutes, left standstill 10 fens Rear potassium chloride and the lithium chloride salt-mixture of removing the surface solidified in the cooling of coming out of the stove behind the clock. The solder piece is added again Heat fusing to 350 ℃ waters the pricker liquid of molten state on angle steel slightly with angle, makes its fast cooling slivering Shape is stand-by.
Example 3: take by weighing 130 gram potassium chloride, 100 grams lithium chlorides and put into alumina crucible, mix, Heat fused to 600 ℃, the pure tin that fused salt is watered 91.95% melts tin fully, under 450 ℃, Zn with 8% joins in the tin liquor of melting, constantly stirs simultaneously, makes the Zn fusing; 0.05% rare earth is fast Ram compression enters in the salt-mixture and Sn-Zn alloy of melting, stirs fusing; Be incubated 30 minutes, left standstill 10 fens Rear potassium chloride and the lithium chloride salt-mixture of removing the surface solidified in the cooling of coming out of the stove behind the clock. The solder piece is added again Heat fusing to 350 ℃ waters the pricker liquid of molten state on angle steel slightly with angle, makes its fast cooling slivering Shape is stand-by.
Example 4: take by weighing 130 gram potassium chloride, 100 grams lithium chlorides and put into alumina crucible, mix, Heat fused to 600 ℃, the pure tin that fused salt is watered 90.9% melts tin fully, under 450 ℃, Zn with 9% joins in the tin liquor of melting, constantly stirs simultaneously, makes the Zn fusing; 0.1% rare earth is fast Ram compression enters in the salt-mixture and Sn-Zn alloy of melting, stirs fusing; Be incubated 30 minutes, left standstill 10 fens Rear potassium chloride and the lithium chloride salt-mixture of removing the surface solidified in the cooling of coming out of the stove behind the clock. The solder piece is added again Heat fusing to 350 ℃ waters the pricker liquid of molten state on angle steel slightly with angle, makes its fast cooling slivering Shape is stand-by.
Below by some charts and example performance after solder of the present invention improves is described. For the ease of than , to contain the tin base leadless soldering-flux of rare earth all be at aforementioned identical with traditional tin base leadless soldering-flux in the present invention Obtain under the part.
In the table 1, example 1-4 is the lead-free brazing that contains rare earth, and example 5,6 is traditional rare earth that do not contain Lead-free brazing. Fusion temperature in the table records with differential thermal analysis.
Table 1 embodiment of the invention and traditional SnZn and SnZnAgBi comparative example 123456 Sn (%) 95.5 93.8 91.95 90.9 91 90 Zn (%) 468994 Re (%) 0.5 0.2 0.05 0.1----Ag (%)----------2 Bi (%)----------4 fusing 204-198 204-198 200-198 198 198 210 temperature (℃)
Annotate: above composition all is weight percentage, and 1-4 be embodiment, example 5, example 6 be traditional do not contain rare SnZn and the SnZnAgBi solder of soil.
As mentioned above, embodiment of the invention 1-4 has the fusion temperature close with traditional SnZn solder, and is suitable Closing the electron trade solder uses.
Below by the improved corrosion resistance of this solder of some marginal datas.
Fig. 1 has represented that the leadless RE that contains of traditional SnZn and SnZnAgBi solder and the present invention's development welds The comparison of the corrosion equilibrium potential of material under the room temperature running water.
As seen from Figure 1, the corrosion equilibrium potential of example 3 of the present invention and example 4 is lower than traditional SnZn solder and SnZnAgBi solder, illustrates that its corrosion resistance improves.
Fig. 2 has represented that the leadless RE that contains of traditional SnZn and SnZnAgBi solder and the present invention's development welds Material under the room temperature running water year corrosion rate comparison.
As seen from Figure 2, the year corrosion rate of example 3 of the present invention and example 4 is lower than traditional SnZn pricker Material and SnZnAgBi solder illustrate that its corrosion resistance improves.
In order to analyze and illustrate the corrosion resistance of this alloy from corrosion mechanism, can be by analyzing solder Anodic polarization curves confirms. That now traditional SnZn solder and the present invention are developed contains the leadless RE weldering The anodic polarization curves of material compares. Shown in Fig. 3,4,5.
Among Fig. 3, the anodic polarization curves of traditional SnZn solder does not have passivation region, and the SnZnAgBi solder a faint passivation region occurred at anodic polarization curves among Fig. 4, and the sun of SnZnRe solder among Fig. 5 There is an obvious passivation region in utmost point polarization curve, its initial corrosion is described after, through passivation, the surface obtains Protection shows corrosion rate and descends.
In sum, adopt the leadless RE that contains of flux total process protective method smelting used among the present invention Its corrosion resistance of solder is better than traditional SnZn and SnZnAgBi solder, and the corrosion equilibrium potential descends corruption Erosion speed obviously reduces.
Claims (5)
1, a kind of tin base leadless soldering-flux that contains rare earth is characterized in that: it is 4～10% Zn that described tin base leadless soldering-flux all contains percentage by weight, 0.05～1% Re, and all the other are Sn, wherein, Re is a mishmetal.
2, the tin base leadless soldering-flux that contains rare earth according to claim 1 is characterized in that: it is 5～10% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.1～1% Re, and all the other are Sn.
3, the tin base leadless soldering-flux that contains rare earth according to claim 1 is characterized in that: it is 6～9% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.05～0.6% Re, and all the other are Sn.
4, the tin base leadless soldering-flux that contains rare earth according to claim 1 is characterized in that: it is 8～9% Zn that available tin base leadless soldering-flux contains percentage by weight, 0.1～0.2% Re, and all the other are Sn.
5, the preparation method who contains the tin base leadless soldering-flux of rare earth according to claim 1 is characterized in that:
(1) with potassium chloride: the salt-mixture of lithium chloride=1.3: 1 (weight ratio) is watering on the tin that is weighing up after 500～600 ℃ of heat fused, treat that tin melts fully after, Zn is joined in the tin liquor of fusion, stir, make the Zn fusing;
(2) rare earth is pressed into rapidly in the salt-mixture and Sn-Zn alloy of fusion, stirs, rare earth is melted fully;
(3) 400～500 ℃ of insulations, treat that alloy mixes after, the salt-mixture that the surface is removed in the back is solidified in the cooling of coming out of the stove after leaving standstill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011312750A CN1161205C (en) | 2001-09-05 | 2001-09-05 | Rare earth-containing tin-base lead-less brazing alloy and its prepn |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011312750A CN1161205C (en) | 2001-09-05 | 2001-09-05 | Rare earth-containing tin-base lead-less brazing alloy and its prepn |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1337293A true CN1337293A (en) | 2002-02-27 |
| CN1161205C CN1161205C (en) | 2004-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011312750A Expired - Fee Related CN1161205C (en) | 2001-09-05 | 2001-09-05 | Rare earth-containing tin-base lead-less brazing alloy and its prepn |
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| Country | Link |
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| CN (1) | CN1161205C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102825396A (en) * | 2012-09-18 | 2012-12-19 | 金华市双环钎焊材料有限公司 | Sn-Zn leadless brazing filler metal containing Pr, Ga and Te |
| CN104668810A (en) * | 2015-01-29 | 2015-06-03 | 苏州天兼新材料科技有限公司 | Novel lead-free welding material and scaling powder preparation method thereof |
| 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 |
| CN106001981A (en) * | 2016-06-23 | 2016-10-12 | 南昌大学 | Lead-free solder added with rare earth carbonate and preparation method |
| WO2020118613A1 (en) * | 2018-12-13 | 2020-06-18 | 北京联金高新科技有限公司 | Sn-zn lead-free solder material and preparation method therefor |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100364712C (en) * | 2004-12-17 | 2008-01-30 | 北京工业大学 | Rare earth Er contained SnZn based leadless solder and its preparation method |
-
2001
- 2001-09-05 CN CNB011312750A patent/CN1161205C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102825396A (en) * | 2012-09-18 | 2012-12-19 | 金华市双环钎焊材料有限公司 | Sn-Zn leadless brazing filler metal containing Pr, Ga and Te |
| CN102825396B (en) * | 2012-09-18 | 2015-06-03 | 金华市双环钎焊材料有限公司 | Sn-Zn leadless brazing filler metal containing Pr, Ga and Te |
| CN104668810A (en) * | 2015-01-29 | 2015-06-03 | 苏州天兼新材料科技有限公司 | Novel lead-free welding material and scaling powder preparation method thereof |
| CN104668810B (en) * | 2015-01-29 | 2016-09-07 | 苏州天兼新材料科技有限公司 | A kind of novel lead-free welding material and the preparation method of scaling powder thereof |
| 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 |
| CN105904115B (en) * | 2016-06-14 | 2018-07-10 | 福建工程学院 | A kind of ZnSn-base high-temperature lead-free soft solder and preparation method thereof |
| CN106001981A (en) * | 2016-06-23 | 2016-10-12 | 南昌大学 | Lead-free solder added with rare earth carbonate and preparation method |
| WO2020118613A1 (en) * | 2018-12-13 | 2020-06-18 | 北京联金高新科技有限公司 | Sn-zn lead-free solder material and preparation method therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1161205C (en) | 2004-08-11 |
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