CN102534347B - Sn-Pb-Zn-Sb alloy and application and preparation method thereof - Google Patents
Sn-Pb-Zn-Sb alloy and application and preparation method thereof Download PDFInfo
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- CN102534347B CN102534347B CN2010106163127A CN201010616312A CN102534347B CN 102534347 B CN102534347 B CN 102534347B CN 2010106163127 A CN2010106163127 A CN 2010106163127A CN 201010616312 A CN201010616312 A CN 201010616312A CN 102534347 B CN102534347 B CN 102534347B
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- 229910001245 Sb alloy Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052718 tin Inorganic materials 0.000 claims abstract description 54
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 238000005266 casting Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 20
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001125 extrusion Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000007872 degassing Methods 0.000 claims abstract description 5
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 5
- 239000010439 graphite Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 52
- CZJCMXPZSYNVLP-UHFFFAOYSA-N antimony zinc Chemical compound [Zn].[Sb] CZJCMXPZSYNVLP-UHFFFAOYSA-N 0.000 claims description 41
- 239000002140 antimony alloy Substances 0.000 claims description 37
- 239000011701 zinc Substances 0.000 claims description 22
- 239000007858 starting material Substances 0.000 claims description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 239000002893 slag Substances 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229910000679 solder Inorganic materials 0.000 abstract description 23
- 239000000919 ceramic Substances 0.000 abstract description 22
- 238000005219 brazing Methods 0.000 abstract description 13
- 229910052745 lead Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000005476 soldering Methods 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses an Sn-Pb-Zn-Sb alloy, which comprises the following components in percentage by mass: 20-50 percent of Pb, 1.0-10 percent of Zn, 0.2-5 percent of Sb and the balance of Sn, belongs to a low-temperature active soft solder and is used for directly brazing ceramic and ceramic or brazing ceramic and metals. A preparation method of the Sn-Pb-Zn-Sb alloy comprises the following steps of: calculating and weighing raw materials including Sn, Pb, Zn and Sb with high purity according the proportion ranges which do not exceed the mass percentage, and placing the raw materials into a crucible; heating by two stages till the raw materials are fully molten; degassing and slagging glycerol and sufficiently stirring; pouring into a graphite die; air-cooling to form a casting ingot; carrying out surface treatment on the casting ingot and placing into a muffle furnace; heating to 110 DEG C, and preserving the temperature for 2h; loading the die and the casting ingot into a preheated extrusion container for stable extrusion; and feeding wires as a finished product into a shaft. The prepared Sn-Pb-Zn-Sb alloy disclosed by the invention is the low-temperature active soft solder, can be used for directly brazing ceramic/ceramic or ceramic/metal and has the advantages of simplifying a process of carrying out metalizing before ceramic brazing and reducing the production cost.
Description
Technical field
The present invention relates to a kind of is the low temperature brazing material of mother metal for glass/ceramic etc., relates in particular to a kind of tin, lead and zinc antimony alloy state silk material solder and preparation method thereof.
Background technology
The glass/ceramic material has high strength, high rigidity, the feature such as corrosion-resistant, is widely applied to the fields such as metallurgy, aerospace, the energy, machinery, automobile, electronics, optics.Pottery is the research emphasis in each field with the interconnection technique of pottery, pottery and metal all the time, is also one of gordian technique of producing ceramic product.Realize that at present the method that pottery is connected with metal has a lot, mainly contain: mechanical connection method, static connection method, hot isostatic pressing method, method for brazing and solid-state diffusion connection method etc.Brazing has the advantages such as joint is reliable, reproducible to be become pottery and is connected the most frequently used method with metal.And the direct method for brazing of reactive metal becomes the emphasis of various countries' research and application especially owing to having the advantages such as suitability is wide, technology is simple, strength of joint is high, reproducible, production cost is relatively low.
Pottery is thermal stresses with another problem of solder bonding metal.The thermal expansivity of pottery is little, with the thermal expansivity of metal, differs larger.When brazing pottery and metal, in joint, can produce unrelieved stress, weaken the mechanical property of joint, also can cause connecting the destruction cracking of rear joint when serious.In order to reduce due to the caused unrelieved stress of the swollen difference of coefficients of line of material, generally employing method has: adopt solder, soft middle layer, the hard metal close with ceramic coefficient of linear expansion to make middle layer, composite interlayer and employing low temperature and be connected etc.
Stupalith mainly contains ionic linkage and covalent linkage, shows highly stable electronics coordination.Make ceramic surface wetting by the metal solder of metallic bond, between solder and pottery, must have chemical reaction to occur.By reaction, make ceramic surface be decomposed to form cenotype, produce chemisorption mechanism, and then form stronger interface binding power.General transition metal can produce and decompose at ceramic surface by chemical reaction, forms the responding layer be comprised of metal and ceramic composite article, and its structure and metallographic phase are same, the wetting metal that can be melted.
Commonly use at present Ti in active solder as active element.It is matrix element that the low temperature active solder generally be take Sn or Pb, as SnAgTi10-4, and solid-liquid temperature 221-300 ℃.Temperature lower than the active solder of 200 ℃ still less.
Summary of the invention
The purpose of this invention is to provide a kind of tin, lead and zinc antimony alloy, can be directly used in the brazing between pottery and pottery, pottery and metal using it as new low temperature active solder, to solve the shortage of the active solder under 200 ℃.
For achieving the above object, the present invention takes following design:
A kind of tin, lead and zinc antimony alloy, its one-tenth is grouped into and mass percent: Pb, 20-50%; Zn, 1.0-10%; Sb, 0.2-5%; Sn, surplus.
Best each constituent mass per-cent of tin, lead and zinc antimony alloy composition for the low temperature active solder is: Pb:36-37%, Zn:3.0-3.5%, Sb:1.0-1.5%, Sn: surplus.To be warming up to fusing through at least two phase process by high purity tin, lead, zinc and the antimony starting material of this ratio range, then the liquid of fusing will fully be stirred at 250 ℃～280 ℃ of temperature, obtain temperature of fusion alloy state solder between 175-185 ℃ after condensation.
Another object of the present invention is to provide purposes of a kind of tin, lead and zinc antimony alloy and preparation method thereof, for processing the low temperature active solder, directly ceramic soldering and pottery or ceramic soldering and metal, considered the thermal stress issues in pottery and solder bonding metal in its preparation method.
For achieving the above object, the present invention takes following design:
A kind of purposes of tin, lead and zinc antimony alloy, as the low temperature active solder, directly ceramic soldering and pottery, or ceramic soldering and metal.
A kind of preparation method of tin, lead and zinc antimony alloy, at first prepare tin, lead and zinc antimony alloy ingot casting, then push as tin, lead and zinc antimony alloy state silk material, and method steps is as follows:
1) by not super ratio range, calculate, weigh standby high purity tin, lead, zinc and antimony starting material, described each composition of raw material mass percent is: Pb, 20-50%; Zn, 1.0-10%; Sb, 0.2-5%; Sn, surplus; And will push and correctly be installed in extrusion machine with mould;
2) metallic tin, lead, zinc and antimony are put into to crucible, heat up in two stages, until starting material all melt;
3) add glycerine degasification slag making in the tin, lead and zinc antimony metal liquid of fusing;
4) continue to heat up, the metal liquid temperature to 250 of controlled melting ℃～280 ℃, fully stir;
5) pour in graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
6) the qualified tin, lead and zinc antimony alloy ingot casting made is placed to retort furnace, be warming up to 110 ℃, be incubated 2 hours; Simultaneously, extrusion mould, container are heated to 110 ℃, are incubated and wait to squeeze;
7) will be incubated ingot casting after the 2 hours container of packing into, and open extrusion machine, and give pressure 1-3MPa, when bar to be extruded touches ingot casting downwards, slowly pressurization, when pressure rises to 9MPa, keep voltage stabilizing;
8) after wire vent, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
Described step 2), in, the amount of putting into of metallic tin, lead, zinc and antimony guarantees that the molten metal after fusing does not overflow crucible and is as the criterion.The detailed process that two steps heat up is: a) power-on, give power 5kw, and preheated crucible and starting material are to 100-150 ℃, 5-10 minute; B) improve power to 20kw, until starting material all melt.
At completing steps 5) after, locate end to end each sampling at the ingot casting obtained and send chemical analysis, molten flow point test; After being rejected to surperficial burr, qualified ingot casting enters into lower program.
Advantage of the present invention is:
1, tin, lead and zinc antimony alloy solder of the present invention is a kind of low temperature active solder, and directly ceramic soldering and pottery, pottery and metal, simplified conventional Ceramic brazing metallization operation before.
2, the tin, lead and zinc antimony alloy solder temperature of fusion that the present invention makes is between 175-185 ℃, is the optimal temperature of ceramic low-temp soldering, so the utmost point is suitable for the soldering with pottery, pottery and metal at the pottery below 200 ℃.
When the tin, lead and zinc antimony alloy 3, made is used as the soldering of pottery and pottery, pottery and metal as the low temperature active solder, can overcome the disadvantageous effect that the thermal stresses in soldering is brought, the good mechanical properties of brazed joint, not easy to crack.
4, preparation method of the present invention has solved poor, the difficult machine-shaping problem of tin, lead and zinc antimony alloy plasticity, can produce the brazing wire that the alloy state is applicable to low temperature brazing.
5, the present invention has filled up the blank that domestic pottery below 200 ℃ is used active medium solder, more can reduce production costs, and economic results in society are remarkable.
Embodiment
Tin, lead and zinc antimony alloy of the present invention becomes to be grouped into and mass percent is: Pb, 20-50%; Zn, 1.0-10%; Sb, 0.2-5%; Sn, surplus.In the soldering with pottery, pottery and metal for pottery below 200 ℃, the optimal components of tin, lead and zinc antimony alloy forms and each constituent mass per-cent is: Pb:36-37%, Zn:3.0-3.5%, Sb:1.0-1.5%, Sn: surplus.The alloy state solder temperature of fusion that this one-tenth is grouped into, between 175-185 ℃, is the optimal temperature of ceramic low-temp soldering.
In the present invention, the most frequently used specification of tin, lead and zinc antimony alloy is thread.The invention provides the preparation method of a kind of tin, lead and zinc antimony alloy (that is alloy state silk material), its concrete grammar step is as follows:
(1) founding: at first prepare tin, lead and zinc antimony alloy ingot casting, method steps is as follows:
1) calculate, weigh for high purity tin, lead, zinc, antimony starting material by not super above-mentioned ratio range; Metallic tin, lead, zinc, antimony are put into to the alumina crucible of certain specification, crucible size how many determines according to feeding intake, and to melt rear molten metal, do not overflow and is as the criterion; Install the extruding mould simultaneously in extrusion machine;
2) a) power-on, give power 5kw, and preheated crucible and starting material are to 100-150 ℃, 5-10 minute; B) improve power to 20kw, until starting material all melt;
3) add glycerine in the tin, lead and zinc antimony metal liquid of fusing, the degasification slag making is processed;
4) continue to heat up, control fluid temperature to 250 ℃～280 ℃, fully stir;
5) the tin, lead and zinc antimony metal liquid stirred is poured in graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
6) each sampling end to end, send chemical analysis and melt the flow point test;
7) will detect qualified tin, lead and zinc antimony alloy ingot casting forwards in next step extruding program.
(2) extruding: the qualified ingot casting that composition, molten flow point are met to technical requirements is pushed, and method steps is as follows:
1) place in retort furnace after the burr of rejecting ingot casting surface, retort furnace is warming up to 110 ℃, be incubated 2 hours; Muff is heated to 110 ℃, is incubated and waits to squeeze;
2) will be incubated ingot casting after 2 hours packs in container;
3) open extrusion machine, give pressure 1-3MPa, when bar to be extruded touches ingot casting downwards, slowly pressurization, when progressively adding to pressure and rising to 9MPa, keep voltage stabilizing, examines filament mouth;
4) after wire vent, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
Below in conjunction with specific embodiment, the present invention is described in further details:
embodiment 1:
Adopt following preparation method to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:20%, and Zn:1%, Sb:0.2%, Sn:78.8%(is called for short SnPbZnSb20-1-0.2).
Concrete preparation method is as follows:
1) press Pb:20%, Zn:1%, Sb:0.2%, the ratio of component of Sn:78.8% is weighed for high purity tin, lead, zinc, antimony starting material; The mould that correct installation is pushed simultaneously;
2) metallic tin, lead, zinc, antimony are put into to alumina crucible;
3) switch power supply, give power 5kw, baking crucible and starting material 5 minutes;
4) improve power to 20kw, until starting material all melt;
5) add glycerine degasification slag making;
6) control fluid temperature to 250 ℃～280 ℃, fully stir;
7) pour in graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
8) chemical analysis, molten flow point test are sent in each sampling end to end;
The qualified ingot casting that 9) will meet technical requirements is rejected its surperficial burr;
10) ingot casting is placed retort furnace, and retort furnace is warming up to 110 ℃, is incubated 2 hours; Muff is heated to 110 ℃, is incubated and waits to squeeze;
11) will be incubated ingot casting after the 2 hours container of packing into, open extrusion machine, give pressure 2MPa, when bar to be extruded touches ingot casting downwards, slowly pressurization;
12) when pressure rises to 9MPa, keep voltage stabilizing, examine filament mouth;
13) after wire vent, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
embodiment 2:
Adopt the described method of embodiment 1 to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:50%, and Zn:10%, Sb:5%, Sn:35%(is called for short SnPbZnSb50-10-5).
embodiment 3:
Adopt the described method of embodiment 1 to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:36%, and Zn:3%, Sb:1%, Sn:60%(is called for short SnPbZnSb36-3-1).
embodiment 4:
Adopt the described method of embodiment 1 to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:37%, and Zn:3.5%, Sb:1.5%, Sn:58%(is called for short SnPbZnSb37-3.5-1.5).
The some variations in addition of the span of each component of above-mentioned tin, lead and zinc antimony alloy do not enumerate herein, therefore that above explanation should be considered as is exemplary, but not in order to limit the protection domain of the present patent application patent.
Concrete location parameter is as following table.
Claims (4)
1. the preparation method of a tin, lead and zinc antimony alloy is characterized in that:
At first prepare tin, lead and zinc antimony alloy ingot casting, then push as tin, lead and zinc antimony alloy state silk material, method steps is as follows:
1) calculate, weigh for high purity tin, lead, zinc and antimony starting material by not super ratio range, described each composition of raw material mass percent is: Pb, 20-50%; Zn, 1.0-10%; Sb, 0.2-5%; Sn, surplus; And will push and correctly be installed in extrusion machine with mould;
2) metallic tin, lead, zinc and antimony are put into to crucible, heat up in two stages, all melt to starting material;
3) add glycerine degasification slag making in the tin, lead and zinc antimony metal liquid of fusing;
4) continue to heat up, the metal liquid temperature to 250 of controlled melting ℃～280 ℃, fully stir;
5) pour in graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
6) the qualified tin, lead and zinc antimony alloy ingot casting made is placed to retort furnace, be warming up to 110 ℃, be incubated 2 hours; Simultaneously, will heat container to 110 ℃, and be incubated and wait to squeeze;
7) will be incubated ingot casting after the 2 hours container of packing into, and open extrusion machine, and give pressure 1-3MPa, when bar to be extruded touches ingot casting downwards, slowly pressurization, when pressure rises to 9MPa, keep voltage stabilizing;
8) after wire vent, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
2. the preparation method of tin, lead and zinc antimony alloy according to claim 1 is characterized in that:
Described step 2), in, the amount of putting into of metallic tin, lead, zinc and antimony guarantees that the molten metal after fusing does not overflow crucible and is as the criterion.
3. the preparation method of tin, lead and zinc antimony alloy according to claim 1 is characterized in that: described step 2), the detailed process that two steps heat up is: a) power-on, give power 5kw, and preheated crucible and starting material are to 100-150 ℃, 5-10 minute; B) improve power to 20kw, until starting material all melt.
4. the preparation method of tin, lead and zinc antimony alloy according to claim 1, is characterized in that: at completing steps 5) after, locate end to end each sampling at the ingot casting obtained and send chemical analysis, the test of molten flow point, after being rejected to surperficial burr, qualified ingot casting enters into lower program.
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| CN2010106163127A CN102534347B (en) | 2010-12-31 | 2010-12-31 | Sn-Pb-Zn-Sb alloy and application and preparation method thereof |
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| CN2010106163127A CN102534347B (en) | 2010-12-31 | 2010-12-31 | Sn-Pb-Zn-Sb alloy and application and preparation method thereof |
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| CN104690439A (en) * | 2013-12-04 | 2015-06-10 | 青岛润鑫伟业科贸有限公司 | Soft solder for copper brazing |
| CN104741819B (en) * | 2013-12-31 | 2018-11-16 | 北京有色金属与稀土应用研究所 | A kind of Pb-Sn-Sb-Ag solder alloy and preparation method thereof |
| CN108188613B (en) * | 2017-11-28 | 2020-06-09 | 深圳市福摩索金属制品有限公司 | Active solder and preparation method and application thereof |
| CN115094267B (en) * | 2022-05-20 | 2023-04-28 | 江苏海瑞电源有限公司 | Lead-based bearing alloy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4887760A (en) * | 1986-08-27 | 1989-12-19 | Kabushiki Kaisha Toshiba | Bonding sheet for electronic component and method of bonding electronic component using the same |
| CN101423907A (en) * | 2007-10-29 | 2009-05-06 | 北京有色金属与稀土应用研究所 | Sn-Ge-As alloy as well as preparation method and use thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4887760A (en) * | 1986-08-27 | 1989-12-19 | Kabushiki Kaisha Toshiba | Bonding sheet for electronic component and method of bonding electronic component using the same |
| CN101423907A (en) * | 2007-10-29 | 2009-05-06 | 北京有色金属与稀土应用研究所 | Sn-Ge-As alloy as well as preparation method and use thereof |
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