CN1052674C - Tin-base active flux for soldering ceramic under coarse vacuum condition - Google Patents
Tin-base active flux for soldering ceramic under coarse vacuum condition Download PDFInfo
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- CN1052674C CN1052674C CN95112026A CN95112026A CN1052674C CN 1052674 C CN1052674 C CN 1052674C CN 95112026 A CN95112026 A CN 95112026A CN 95112026 A CN95112026 A CN 95112026A CN 1052674 C CN1052674 C CN 1052674C
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- welding
- tin
- solder
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- base active
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Abstract
The present invention provides a tin-base active filler metal for welding ceramics under a coarse vacuum condition. The filler metal is basically composed of 1 to 10 of active metal and balance of tin by atomic percentage, wherein the active metal is titanium, zirconium, hafnium, vanadium or the composition thereof. The present invention is characterized in that the filler metal also contains 2 to 30 of volatile component which is plumbum, zinc, phosphorus, manganese or the composition thereof. The Sn-base active filler metal provided by the present invention can be used in coarse vacuum provided by a mechanical pump, which is convenient to popularize and use.
Description
The invention belongs to extraordinary welding technology field, specifically just provide a kind of extraordinary active solder, it is applicable to the welding of implementing pottery and ceramic welding or pottery and metal under the coarse vacuum condition that oil-sealed rotary pump provides, does not need to carry out in advance metalized on welding pre-ceramic surface.
Since the nearly period, because the joint efforts of various countries scientific circles and industrial quarters make traditional ceramic material property that the variation of essence take place, the production of fine ceramics material has become a new industry department, and its product has entered the practicability stage.Yet when this new material is changed in the process of actual product manufacturing by investigation of materials, preparation, as other material, reliable interconnection technique is one of key problem in technology that must at first be solved.
Existing multiple metal and ceramic interconnection technique, as mechanical connection, organic bonding, inorganic adhesive, the solid-state reaction welding, friction welding (FW), laser weld, behind the ceramic surface metallization, soldering indirectly, direct soldering of reactive metal method or the like.Each technology all has certain scope of application and pluses and minuses, and is unreliable as mechanical connection, and makes structure complicated, and the temperature tolerance of organic bonding is very low, and the adhesive strength of inorganic adhesive is low, and sealing difference and be easy to hydrolysis.The sweating heat stress of solid-state reaction welding is very big and welding cost is high, productivity ratio is low, friction welding (FW) only is applicable to specific material fit and must is the part of simple shape, laser weld only is applicable to the welding between the chloride pottery of definite fusing point, soldering has not only increased the complexity of production technology behind the ceramic surface metallization, and because the fluctuation of surface metal metallization processes, waste product in the middle of being easy to produce finally increases defectives such as production cost.As a comparison, it is generally acknowledged for joint quality and have relatively high expectations, and under the bigger situation of production lot, the direct soldering tech of reactive metal method has competitiveness most, its topmost advantage is the productivity ratio height, and the wide accommodation quality of connection is reliable, and comprehensive production cost is lower, and the core of this technology provide a kind of can be directly wetting on ceramic surface, the active metallic soldering material of sprawling and adhering to.
There is the active metallic soldering material of several different systems to be used for ceramic welding, the auri or the palladium based active solder that provide as the patent EP of the European Community 0104623 (1983), the money base active solder that the clear 62-16896 of Japan Patent (1987) provides, a kind of anti-oxidation active metallic soldering materials that copper-based active solder that BP GB2066291 (1981) provides and Chinese patent ZL 92106103.X (1995) provide etc., these active metallic soldering materials are under high vacuum condition (＜10
-4Toor) the effectively wetting and multiple ceramic material of welding of energy, yet the common drawback of these active solders is that the fusing point of solder itself is higher, welding finishes in the later cooling procedure, because the thermal expansion difference of metal and ceramic material, to form very big welding residual thermal stress in the welding point, when this residual stress is too high, usually cause near the ceramic material of welding point to ftracture voluntarily.
In order to reduce sweating heat stress, be necessary to develop a kind of low-melting active metallic soldering material, because metal can not transmit stress before solidifying fully, therefore the final fusing point of solder is low more, mean that then the postwelding residual thermal stress is more little, this is particularly important to the lower ceramic material of the welding of success some self intensity, and it is the low melting point active solder such as the Chinese patent ZL92106127.7 (1995) of basic composition that existing at present several patented technologies provide with tin; German patent DE 3641679A1 (1987) and the flat 1-95893 of Japan Patent (1989), the solder prescription that these patented technologies provide generally is made up of three kinds of compositions, promptly
(1) basic composition Sn
(2) active element Ti, Zr or Hf
(3) the 3rd component A g, Cu, Ni, In
This low melting point active solder can be successful welding conventional art some large-size ceramic elements of being difficult to weld, it also can weld some low-intensity function ceramics very responsive to thermal stress simultaneously.Yet the common shortcoming of these active solders is that welding generally requires in higher vacuum (＜10
-4Toor) carry out under, this just means that welding requires to use expensive welding equipment in producing, and consume more time and be used to obtain vacuum and destroy vacuum, causes the bad grade of welding quality to cause high production cost thus by equipment gas leakage.
The object of the present invention is to provide a kind of Sn based active solder that can under coarse vacuum condition, use.
The invention provides a kind of tin-base active solder of welding ceramics, by (atomic percent)
Reactive metal 1～10
Volatile element 2～30
The tin surplus
Form, wherein reactive metal refers to the compound of titanium, zirconium, hafnium, vanadium or them, and volatile element refers to lead, zinc, phosphorus, manganese or theirs is compound.
Also provide the tin-base active solder of another kind of welding ceramics among the present invention, by (atomic percent)
Reactive metal 1～10
Volatile element 2～30
The 3rd constituent element 1～30
The tin surplus
Form, wherein reactive metal refers to the compound of titanium, zirconium, hafnium, vanadium or them, and volatile element refers to the compound of lead, zinc, phosphorus, manganese or them, and the 3rd constituent element refers to silver, copper, nickel, indium or theirs is compound.
Active solder provided by the invention can select a kind of method of common smelting to carry out alloying, with conventional processing method solder is made suitable shape of product then, as solder sheet or solder wire etc.
In general, the effect of parent metal tin is to guarantee that solder has lower final fusing point, to reduce welding stress; The effect of reactive metal is by they interfacial reactions with pottery, reaches to make active solder wetting and purpose of adhering on pottery; The effect of the 3rd constituent element is an intensity of improving and adjust active solder, the comprehensive condition of other of wetability and solder; Essence of the present invention is to add the higher volatile element of some vapour pressures in original Sn based active solder prescription, the characteristic of utilizing these elements at high temperature to volatilize strongly, destroy the established continuous oxidation film layer in liquid metal surface, make fresh active metallic soldering material contact concurrent biochemical reaction with ceramic surface, reach the purpose of under black vacuum, implementing ceramic welding.Compare with original technology, the topmost advantage of the present invention is to use under coarse vacuum condition, and this black vacuum can be obtained (10 by the standard machinery pump
-1-10
-2Torr) and the general medium vacuum degree (10 that provides by oil diffusion pump of requiring of original technology
-4-10
-5Torr), the present invention has not only oversimplified the complexity of welding equipment of the requirement of ceramic welding greatly like this, and reduced greatly for obtain high vacuum and for take out soldering part destroy vacuum the production time that must expend.Therefore advantage provided by the invention not only helps this technology implements use in common factory, and will save production cost greatly, improve the quality of product, owing to adopt base metals such as lead, zinc to carry out alloying, also help further to reduce the manufacturing cost of solder itself in addition.Below by embodiment in detail the present invention is described in detail.
Embodiment 1
Preparation 5%Cu, 5%Ti, 5%Zn, all the other are the active solder of Sn, adopt tungsten electrode argon shield method of smelting to carry out alloying, adopt electromagnetic field to stir in the fusion process, to guarantee the alloy composition homogenising, the cold rolling gradually one-tenth solder of cooling back gradation sheet is standby.Sialon ceramic rod end face to be welded through careful grind and clean after, place on the weld jig, press Sialon/ solder/Sialon assembled in sequence after, these anchor clamps are placed a conventional vacuum stove, seal furnace chamber after, vacuumize with oil-sealed rotary pump, reach (10
-2Torr) after the vacuum, pottery and solder are heated, be warming up to 900 ℃ after, be incubated 20 minutes, close heating power supply then, and with stove cooling, be chilled to room temperature after, obtain the welding point that is connected firmly.
Embodiment 2
Preparation 3%Ag, 4%Ti, 2%Hf, all the other are the active solder of Sn for 25%Pb, adopt to prepare solder as embodiment 1 described program, and implement welding, ceramic material is barium titanate ceramics vacuum 0.1 Torr, has obtained firm welding point after the cooling.
Embodiment 3
This system 10%Cu, 2%Ti, 2%Zr, all the other are the active solder of Sn for 2%P, adopt the program shown in embodiment 1 to prepare solder, and implement welding, material is 10 for aluminium oxide ceramics vacuum
-1Torr after the cooling, has obtained firm welding point.
Embodiment 4
Preparation 3%Cu, 3%Ag, 4%Hf, 25%Pb, all the other are the active solder of Sn for 5%Zn, adopt the program shown in embodiment 1 to prepare solder and implement welding, and material is a silicon nitride ceramics, and vacuum is 10
-2After the Torr cooling, obtained firm welding point.
Embodiment 5
Preparation 1%Ni, 3%Cu, 2%Ti, 1.5%Zr, 15%Pb, all the other are the active solder of Sn for 2%Mn, adopt the program shown in embodiment 1 to prepare solder and implement welding, material is a silicon carbide ceramics, and vacuum has obtained firm welding point after being the 0.1Torr cooling.
Embodiment 6
Preparation 5%Ti, all the other are the active solder of Sn for 10%Pb, adopt the program shown in embodiment 1 to prepare solder and implement welding, and material is the Sialon pottery, and vacuum is 0.1Torr, has obtained firm welding point after the cooling.
Embodiment 7
Preparation 4%Ti, 2%Hf, all the other are the active solder of Sn for 20%Pb, adopt the program shown in embodiment 1 to prepare solder and implement welding, and material is an aluminium oxide ceramics, and vacuum is 0.1Torr, has obtained firm welding point after the cooling.
Embodiment 8 and comparative example
(experimental condition: Sialon/Sialon pottery, 900 ℃ * 30min, four-point bending intensity
| Alloy composition | Welding vacuum | |
| 9.2Toor | 8.1Toor | |
| Original technology Sn-5Cu-5Ti Sn-5Cu-5Ti-25Pb of the present invention | 25-47MPa does not burn-on | 57-94MPa does not burn-on |
Claims (2)
1. the tin-base active solder of a welding ceramics is by (atomic percent)
Reactive metal 1～10
Volatile element 2～30
The tin surplus
Form, wherein reactive metal refers to the compound of titanium, zirconium, hafnium, vanadium or them, and volatile element refers to lead, zinc, phosphorus, manganese or theirs is compound.
2. the tin-base active solder of a welding ceramics is by (atomic percent)
Reactive metal 1～10
Volatile element 2～30
The 3rd constituent element 1～30
The tin surplus
Form, wherein reactive metal refers to the compound of titanium, zirconium, hafnium, vanadium or them, and volatile element refers to the compound of lead, zinc, phosphorus, manganese or them, and the 3rd constituent element refers to silver, copper, nickel, indium or theirs is compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95112026A CN1052674C (en) | 1995-09-27 | 1995-09-27 | Tin-base active flux for soldering ceramic under coarse vacuum condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95112026A CN1052674C (en) | 1995-09-27 | 1995-09-27 | Tin-base active flux for soldering ceramic under coarse vacuum condition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1146390A CN1146390A (en) | 1997-04-02 |
| CN1052674C true CN1052674C (en) | 2000-05-24 |
Family
ID=5079250
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95112026A Expired - Fee Related CN1052674C (en) | 1995-09-27 | 1995-09-27 | Tin-base active flux for soldering ceramic under coarse vacuum condition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052674C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430178C (en) * | 2006-11-23 | 2008-11-05 | 太仓市南仓金属材料有限公司 | Lead-free anti-oxidation alloy of lead-free soldering flux, prepn. method and use thereof |
| CN101214589B (en) * | 2008-01-14 | 2010-06-16 | 哈尔滨工业大学 | Multi-component leadless solder |
| CN101559507B (en) * | 2009-04-17 | 2011-05-11 | 中国航空工业第一集团公司北京航空材料研究院 | Method for adopting copper-based solder to repair titanium alloy castings by welding |
| CN101987402B (en) * | 2010-11-30 | 2012-09-05 | 哈尔滨工业大学 | Method for brazing Ti2AlC ceramics and Cu with Cu-Sn-Ti solder |
| CN102319962B (en) * | 2011-08-24 | 2013-04-24 | 哈尔滨工业大学 | Preparation method of Sn-Zn-Ti activated brazing filler metal with melting point lower than 600 DEG C |
| CN102492367B (en) * | 2011-12-07 | 2013-08-14 | 天津大学 | Low-melting-point metal adhesive and diamond wire saw obtained by metal adhesion |
| CN102848094B (en) * | 2012-06-08 | 2015-05-13 | 浙江吉利汽车研究院有限公司杭州分公司 | Sn-Cu-based environment-friendly solder containing Zr and preparation method thereof |
| CN104710115B (en) * | 2013-12-11 | 2018-03-02 | 中国航空工业第六一八研究所 | A kind of method for forming welding substrate on devitrified glass surface |
| EP3106447B1 (en) * | 2014-02-12 | 2019-04-24 | Mitsubishi Materials Corporation | Copper-ceramic bonded body and power module substrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5524720A (en) * | 1978-08-10 | 1980-02-22 | Asahi Glass Co Ltd | Solder for hard-to-solder material |
| CN1077151A (en) * | 1992-04-11 | 1993-10-13 | 中国科学院金属研究所 | The Sn base active medium solder of weldable ceramic |
| CN1027797C (en) * | 1992-03-25 | 1995-03-08 | 中国科学院金属研究所 | Anti-oxidation active metallic soldering material for welding ceramics |
-
1995
- 1995-09-27 CN CN95112026A patent/CN1052674C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5524720A (en) * | 1978-08-10 | 1980-02-22 | Asahi Glass Co Ltd | Solder for hard-to-solder material |
| CN1027797C (en) * | 1992-03-25 | 1995-03-08 | 中国科学院金属研究所 | Anti-oxidation active metallic soldering material for welding ceramics |
| CN1077151A (en) * | 1992-04-11 | 1993-10-13 | 中国科学院金属研究所 | The Sn base active medium solder of weldable ceramic |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1146390A (en) | 1997-04-02 |
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