CN102534347A - 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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- CN102534347A CN102534347A CN2010106163127A CN201010616312A CN102534347A CN 102534347 A CN102534347 A CN 102534347A CN 2010106163127 A CN2010106163127 A CN 2010106163127A CN 201010616312 A CN201010616312 A CN 201010616312A CN 102534347 A CN102534347 A CN 102534347A
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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 glass/ceramic etc. that is used for and be the low temperature brazing material of mother metal, relate in particular to a kind of tin, lead and zinc antimony alloy attitude silk material solder and preparation method thereof.
Background technology
The glass/ceramic material has HS, high firmness, characteristic such as corrosion-resistant, is widely applied to 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, also is 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.Soldering connects advantages such as having joint is reliable, good reproducibility becomes the ceramic the most frequently used method that is connected with metal.And the direct method for brazing of reactive metal especially because have that suitability is wide, technology is simple, strength of joint is high, advantage, the emphasis that becomes various countries' research and use such as good reproducibility, production cost are relatively low.
Pottery is a thermal stresses with another problem of solder bonding metal.The thermal expansivity of pottery is little, differs bigger with the thermal expansivity of metal.When soldering connects pottery with metal, can produce unrelieved stress in the joint, weaken the mechanical property of joint, also can cause connecting the destruction cracking of back joint when serious.In order to reduce because line of material expands the caused unrelieved stress of difference of coefficients, 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 by the metal solder wetting of metallic bond, between solder and pottery, must have chemical reaction to take place.Make ceramic surface be decomposed to form cenotype through reaction, produce chemisorption mechanism, and then form stronger interface binding power.General transition metal can produce at ceramic surface through chemical reaction and decompose, and forms the responding layer of being made up of metal and ceramic composite article, its structure and metallographic phase together, the wetting metal that can be melted.
Use Ti at present in the active solder always as active element.The low temperature active solder is a matrix element with Sn or Pb generally, like SnAgTi10-4, and 221-300 ℃ of solid-liquid temperature.Temperature be lower than 200 ℃ active solder still less.
Summary of the invention
The purpose of this invention is to provide a kind of tin, lead and zinc antimony alloy, it can directly be used for pottery and ceramic, pottery as new low temperature active solder be connected, to solve the shortage of the active solder under 200 ℃ with soldering between the metal.
For realizing above-mentioned purpose, the present invention takes following plan:
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 the constituent mass per-cent of tin, lead and zinc antimony alloy composition that is used 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, the liquid with fusing fully stirs down for 250 ℃～280 ℃ in temperature again, obtains temperature of fusion alloy attitude solder between 175-185 ℃ after the condensation.
Another object of the present invention provides purposes of a kind of tin, lead and zinc antimony alloy and preparation method thereof; Be used to process the low temperature active solder; Directly ceramic soldering and pottery or ceramic soldering and metal have been considered the thermal stress issues in pottery and the solder bonding metal in its preparation method.
For realizing above-mentioned purpose, the present invention takes following plan:
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 prepares tin, lead and zinc antimony alloy ingot casting, and extruding is tin, lead and zinc antimony alloy attitude silk material again, and method steps is following:
1) calculate by not ultra ratio range, weigh high purity tin, lead, zinc and antimony starting material fully, said 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 the extrusion machine with mould;
2) metallic tin, lead, zinc and antimony are put into crucible, heat up in two stages, all melt until starting material;
3) in the tin, lead and zinc antimony metal liquid of fusing, add glycerine degasification slag making;
4) continue to heat up, control molten metal fluid temperature to 250 ℃～280 ℃ fully stirs;
5) pour in the graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
The qualified tin, lead and zinc antimony alloy ingot casting that 6) will make is placed retort furnace, is warming up to 110 ℃, is incubated 2 hours; Simultaneously, extrusion mould, container are heated to 110 ℃, insulation is waited 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 touched ingot casting downwards, slowly pressurization when treating that pressure rises to 9MPa, kept voltage stabilizing;
8) treat wire vent after, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
Described step 2) in, the molten metal after the amount of putting into of metallic tin, lead, zinc and antimony is guaranteed to melt does not overflow crucible and is as the criterion.The detailed process that two steps heated 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, all melt until starting material.
At completing steps 5) after, locate each sampling end to end at the ingot casting that obtains and send chemical analysis, molten flow point test; Enter into down program after qualified ingot casting rejected surperficial burr.
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 have been simplified conventional ceramic soldering metallization operation before.
2, the tin, lead and zinc antimony alloy solder temperature of fusion that makes of the present invention is between 175-185 ℃, is the optimal temperature of ceramic low temperature soldering, so the utmost point is suitable in the soldering of the pottery below 200 ℃ with pottery, pottery and metal.
When the tin, lead and zinc antimony alloy that 3, makes 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 the soldering is brought, the good mechanical properties of brazed joint, not easy to crack.
4, preparation method of the present invention has solved tin, lead and zinc antimony alloy bad plasticity, difficult machine-shaping problem, can produce the brazing wire that the alloy attitude is applicable to low temperature brazing.
5, the present invention has filled up domestic ceramic blank with active medium solder below 200 ℃, 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.Be used for the soldering of pottery below 200 ℃ with pottery, pottery and metal, the optimal components of tin, lead and zinc antimony alloy is formed and each constituent mass per-cent is: Pb:36-37%, Zn:3.0-3.5%, Sb:1.0-1.5%, Sn: surplus.The alloy attitude solder temperature of fusion that this one-tenth is grouped into is the optimal temperature of ceramic low temperature soldering between 175-185 ℃.
The most frequently used specification of tin, lead and zinc antimony alloy is thread among the present invention.The invention provides the preparation method of a kind of tin, lead and zinc antimony alloy (that is alloy attitude silk material), its concrete grammar step is following:
(1) founding: at first prepare tin, lead and zinc antimony alloy ingot casting, method steps is following:
1) by not ultra above-mentioned ratio range calculating, weigh high purity tin, lead, zinc, antimony starting material fully; Metallic tin, lead, zinc, antimony are put into the alumina crucible of certain specification, and what confirm crucible size according to feeding intake, and do not overflow and are as the criterion to melt the back molten metal; In extrusion machine, install simultaneously extruding and use mould;
2) a) power-on is given power 5kw, and preheated crucible and starting material are to 100-150 ℃, 5-10 minute; B) improve power to 20kw, all melt until starting material;
3) in the tin, lead and zinc antimony metal liquid of fusing, add glycerine, the degasification slag making is handled;
4) continue to heat up, controlled liq temperature to 250 ℃～280 ℃ fully stirs;
5) the tin, lead and zinc antimony metal liquid that stirs is poured in the graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
6) each sampling is end to end sent chemical analysis and is melted the flow point test;
7) will detect qualified tin, lead and zinc antimony alloy ingot casting forwards in next step the extruding program.
(2) extruding: the qualified ingot casting that composition, molten flow point are met technical requirements pushes, and method steps is following:
1) places in the retort furnace behind the burr of rejecting ingot casting surface, retort furnace is warming up to 110 ℃, be incubated 2 hours; Muff is heated to 110 ℃, and insulation is waited to squeeze;
2) will be incubated ingot casting after 2 hours packs in the container;
3) open extrusion machine, give pressure 1-3MPa, when bar to be extruded touched ingot casting downwards, slowly pressurization when progressively adding to pressure and rising to 9MPa, kept voltage stabilizing, examines filament mouth;
4) treat wire vent after, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
Below in conjunction with specific embodiment the present invention is explained 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%, Zn:1%, Sb:0.2%, Sn:78.8% (being called for short SnPbZnSb20-1-0.2).
Concrete preparation method is following:
1) press Pb:20%, Zn:1%, Sb:0.2%, the ratio of component of Sn:78.8% weigh and are equipped with high purity tin, lead, zinc, antimony starting material; The correct simultaneously mould that extruding is installed;
2) metallic tin, lead, zinc, antimony are put into alumina crucible;
3) switch power supply is given power 5kw, baking crucible and starting material 5 minutes;
4) improve power to 20kw, all melt until starting material;
5) add glycerine degasification slag making;
6) controlled liq temperature to 250 ℃～280 ℃ fully stirs;
7) pour in the 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 ℃, and insulation is waited 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;
When 12) treating that pressure rises to 9MPa, keep voltage stabilizing, examine filament mouth;
13) treat wire vent after, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
Embodiment 2:
Adopt embodiment 1 described method to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:50%, Zn:10%, Sb:5%, Sn:35% (being called for short SnPbZnSb50-10-5).
Embodiment 3:
Adopt embodiment 1 described method to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:36%, Zn:3%, Sb:1%, Sn:60% (being called for short SnPbZnSb36-3-1).
Embodiment 4:
Adopt embodiment 1 described method to prepare the tin, lead and zinc antimony alloy, its component and mass percent are: Pb:37%, Zn:3.5%, Sb:1.5%, Sn:58% (being called for short SnPbZnSb37-3.5-1.5).
The in addition some variations of the span of each component of above-mentioned tin, lead and zinc antimony alloy are not enumerated here one by one, so above explanation should be regarded as exemplary, but not the protection domain of applying for a patent in order to restriction the present invention.
Concrete location parameter such as following table.
Claims (8)
1. tin, lead and zinc antimony alloy, it is characterized in that: its one-tenth is grouped into and mass percent is Pb, 20-50%; Zn, 1.0-10%; Sb, 0.2-5%; Sn, surplus.
2. tin, lead and zinc antimony alloy according to claim 1 is characterized in that: optimal components is formed and each constituent mass per-cent is: Pb:36-37%, Zn:3.0-3.5%, Sb:1.0-1.5%, Sn: surplus.
3. tin, lead and zinc antimony alloy according to claim 2; It is characterized in that: will be by the high purity tin of this ratio range, lead, zinc and antimony starting material through at least two stage temperature-rise periods to material melts; Liquid with fusing fully stirs down for 250 ℃～280 ℃ in temperature again, obtains temperature of fusion alloy attitude solder between 175-185 ℃ after the condensation.
4. the purposes of the said tin, lead and zinc antimony alloy of claim 1 is characterized in that: as the low temperature active solder, and directly ceramic soldering and pottery, or ceramic soldering and metal.
5. the preparation method of the said tin, lead and zinc antimony alloy of claim 1 is characterized in that:
At first prepare tin, lead and zinc antimony alloy ingot casting, extruding is tin, lead and zinc antimony alloy attitude silk material again, and method steps is following:
1) by not ultra ratio range calculating, weigh high purity tin, lead, zinc and antimony starting material fully, said 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 the extrusion machine with mould;
2) metallic tin, lead, zinc and antimony are put into crucible, heat up in two stages, all melt to starting material;
3) in the tin, lead and zinc antimony metal liquid of fusing, add glycerine degasification slag making;
4) continue to heat up, control molten metal fluid temperature to 250 ℃～280 ℃ fully stirs;
5) pour in the graphite mo(u)ld, air cooling forms tin, lead and zinc antimony alloy ingot casting;
The qualified tin, lead and zinc antimony alloy ingot casting that 6) will make is placed retort furnace, is warming up to 110 ℃, is incubated 2 hours; Simultaneously, will heat container to 110 ℃, insulation is waited 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 touched ingot casting downwards, slowly pressurization when treating that pressure rises to 9MPa, kept voltage stabilizing;
8) treat wire vent after, observe wire vent speed, constantly regulate pressure, keep welding wire evenly to extrude.
6. the preparation method of tin, lead and zinc antimony alloy according to claim 5 is characterized in that:
Said step 2) in, the molten metal after the amount of putting into of metallic tin, lead, zinc and antimony is guaranteed to melt does not overflow crucible and is as the criterion.
7. the preparation method of tin, lead and zinc antimony alloy according to claim 5 is characterized in that: said step 2), the detailed process that two steps heated 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, all melt until starting material.
8. the preparation method of tin, lead and zinc antimony alloy according to claim 5 is characterized in that: at completing steps 5) after, locate each sampling end to end at the ingot casting that obtains and send chemical analysis, the test of molten flow point, after being rejected surperficial burr, qualified ingot casting enters into down program.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104741819A (en) * | 2013-12-31 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Pb-Sn-Sb-Ag alloy brazing filler metal and manufacturing method thereof |
| CN108188613A (en) * | 2017-11-28 | 2018-06-22 | 深圳市福摩索金属制品有限公司 | A kind of active solder and its preparation method and application |
| CN115094267A (en) * | 2022-05-20 | 2022-09-23 | 江苏海瑞电源有限公司 | Lead-based bearing alloy for high-performance bearing and preparation method thereof |
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| 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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2010
- 2010-12-31 CN CN2010106163127A patent/CN102534347B/en active Active
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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104741819A (en) * | 2013-12-31 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Pb-Sn-Sb-Ag alloy brazing filler metal and manufacturing method thereof |
| 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 |
| CN108188613A (en) * | 2017-11-28 | 2018-06-22 | 深圳市福摩索金属制品有限公司 | A kind of active solder and its preparation method and application |
| 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 |
| CN115094267A (en) * | 2022-05-20 | 2022-09-23 | 江苏海瑞电源有限公司 | Lead-based bearing alloy for high-performance bearing and preparation method thereof |
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| CN102534347B (en) | 2013-12-11 |
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