CN1196563C - Ag solder for welding and soldering method using it - Google Patents
Ag solder for welding and soldering method using it Download PDFInfo
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- CN1196563C CN1196563C CN 02106267 CN02106267A CN1196563C CN 1196563 C CN1196563 C CN 1196563C CN 02106267 CN02106267 CN 02106267 CN 02106267 A CN02106267 A CN 02106267A CN 1196563 C CN1196563 C CN 1196563C
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Abstract
Provided is an Ag brazing filler metal in which solidus temperature and liquidus temperature lie in the range of 800 to 900 deg.C. The Ag brazing filler metal for joining has a composition consisting of, by weight, 1.0 to 10.0% tin (Sn) and 2.5 to 10% copper (Cu), and the balance Ag. The solidus temperature of the Ag brazing filler metal is >=800 deg.C, and its liquidus temperature is 900 deg.C. If required, the brazing filler metal can contain <=6.0% manganese (Mn), 0.1 to 2.5% nickel (Ni) or both of them.
Description
Technical field
The present invention relates to Ag solder for welding and use its method for welding, particularly its solidus temperature more than 800 ℃, liquidus temperature below 900 ℃, the Ag scolder of cheap and applied widely, excellent weldability.
Technical background
With the existing Ag scolder (JIS, Z3261) of Ag-Cu alloy as principal component, its brazing temperature range is 620～900 ℃, and solidus temperature is 605～780 ℃.This Ag-Cu scolder is widely used in the metal solder, for example, to the welding between weld metal, the stainless steel on the ceramic substrate, on stainless steel soldering copper (Cu) goods, or the welding between the copper spare etc.
These existing Ag-Cu scolders, low according to its kind, high 605 ℃ of beginning fusions, 780 ℃ of beginning fusions.
When having only a welding position, though more satisfactory with this existing Ag scolder,, according to assembling procedure, when different time welding position, number place, use several different scolders of each fusing point, carry out weld job successively.Such soldering is called the substep soldering, or the soldering of multistage substep.Usually at first use the high scolder of fusing point, a part welding is lived.Subsequently, weld other position with low-melting scolder again.For example, at first using the Ni of 1000 ℃ of fusing points is scolder, carry out soldering after, other positions are again with the welding of above-mentioned Ag-Cu scolder.
Yet, using Ni is that high melting point solder welds step by step, when being the very high member of hear resistance for the member of welding object, do not have problems, but for the parts that are easy to soften in brazing temperature, when for example carrying the welding of copper (Cu) member made on substrate, in weld job, the mother metal of Cu member made takes place softening, the softening characteristic that can influence equipment of such crystallization.
Than the existing Ag melt solder temperature that with BAg-8 is representative high and also have the softening scolder that not have melt temperature that influences of the mother metal of soldered parts, in other words, its solidus temperature more than 800 ℃, liquidus temperature is at the Ag scolder below 900 ℃, be most popular, but, the current Ag-Cu scolder that does not also have this temperature range.
In the scolder outside the Ag-Cu system, as the scolder of 800-900 ℃ of melt temperature scope, the Pd that use palladium (Pd) is arranged be scolder (JIS, Z3267), use the Au of gold (Au) be scolder (JIS, Z3266).Yet, Pd is that scolder and Au are scolder, with the Ag scolder relatively, the material price is high, exists the great problem of manufacturing cost.
And then, as other problem, using existing Ag scolder, welding as pre-treatment, must be implemented plating Ni (nickel) to soldered member when having the member of passivity tunicle on the surfaces such as stainless steel component.This is because under the influence of passive film, can not guarantee surperficial autgmentability, or the autgmentability of scolder.That is, when using existing scolder, need plate the Ni part, remainder needs other operations, causes manufacturing cost to increase.Though also considered to use the existing Ag scolder (JIS) that has been pre-mixed Ni to replace plating Ni, the solidus temperature of BAg-13a and BAg-21 is below 800 ℃, when low temperature brazing, and fusion instability more sometimes.In addition, the solidus temperature of BAg-23 is considerably beyond 900 ℃, and it is too high that brazing temperature becomes, very undesirable.
And then as other problems, in the existing Ag-Cu scolder, with the nonoverlapping 2 kinds of Ag scolders of brazing temperature range, for example solidus temperature be 780 ℃ with liquidus temperature be lower than 780 ℃ (for example, BAg-3) make up and when carrying out the substep soldering, existence can not be carried out vacuum treated problem.Low-melting Ag-Cu contains zinc (Zn) and cadmium (Cd) in the composition of scolder, when this scolder is used for soldering in vacuum chamber, can forms in the vacuum chamber and pollute, so have to carry out soldering in atmospheric environment.
When handling in atmospheric environment, because soldered member is surperficial oxidized, so on one side must weld with the surperficial oxide of flux removal, also need to remove flux on one side after welding, whole soldered thing must clean.Therefore, when increasing welding sequence, also have influence on environmental problem.
And then, in the process of welding object microminiaturizations such as electronic unit, when needing the welding of micro-member and need the member of hermetic seal also a lot, as vacuum tube, vacuum sphere etc.In so airtight soldering and small soldering, need fully to enter the impregnability in the minim gap.
Summary of the invention
The 1st purpose of the present invention provide a kind of solidus temperature more than 800 ℃, liquidus temperature is at the new A g scolder below 900 ℃.
The 2nd purpose of the present invention provides before a kind of welding, do not need soldered thing (stainless steel, pottery etc.) is plated the Ag scolder that Ni handles and has abundant autgmentability and impregnability.
The 3rd purpose of the present invention provides a kind ofly both can be handled in atmosphere, can carry out the Ag scolder of soldering again in vacuum chamber.
The 4th purpose of the present invention provides the welding of high member of a kind of suitable air-tightness and small electric subassembly and the Ag scolder with impregnability.
Such Ag scolder about 800 ℃ of beginning fusions, finishes about 900 ℃ of fusions.Therefore, by being that 620 ℃-800 ℃ existing Ag scolder and brazing temperature makes up at the existing Ni scolder more than 1000 ℃ with brazing temperature, can realize many substeps solderings for several times.
The material of new A g scolder of the present invention and welding object is irrelevant, can be as the scolder that welds in extensive fields.
In order to achieve the above object, the present invention 1 welding expects that with Ag tin (Sn), the copper (Cu) of 2.5-10 weight %, remainder by 1.0-10.0 weight % are that silver (Ag) constitutes.
The solidus temperature of this Ag scolder is more than 800 ℃, and liquidus temperature is below 900 ℃.Basically be the eutectic that has utilized Ag and Cu, be taken as the scope of 2.5-10 weight % (following according to circumstances only adopt " % "), make the melt temperature scope of Ag scolder roughly be set in scope near 800 ℃-900 ℃ by composition with Cu.To wherein adding Sn, can reduce liquidus temperature again, the melt temperature of Ag welding can be controlled in 800 ℃-900 ℃ the target zone.Sn has the effect of improving autgmentability, even welding thing surface has the situation of passivity tunicle, also there is no need to implement plating Ni as pre-treatment.
The Cu amount is difficult to the liquidus temperature of Ag scolder is controlled at below 900 ℃ below 2.5%, if more than 10%, is difficult to solidus temperature is controlled at more than 800 ℃.
Sn amount is below 1.0%, and the effect that the liquidus temperature of Ag scolder is controlled at below 900 ℃ can reduce.Sn amount surpasses 10.0%, can increase fragility, impairs the ductility as the matrix of principal component with Ag and Cu.
The cost of above-mentioned Ag scolder is very low, and impregnability is very good, can bring into play good weldability.
The present invention 2 Ag solder for welding by the following manganese (Mn) of copper (Cu), the 6.0 weight % of the tin (Sn) of 1.0-10.0 weight %, 2.5-10 weight %, all the other are formed for silver-colored (Ag).By adding the Mn below 6.0%, can improve the intensity of (Ag) scolder, also improved wetability or autgmentability simultaneously to stainless steel and pottery.Mn content is when 0.3-6.0%, and autgmentability is good especially.The impregnability of especially above-mentioned Ag scolder self is very good, but it doesn't matter with Mn content, even Mn content is lower than 0.3%, Ag scolder as a whole also can be brought into play suitable intensity and good weldability.When Mn amount reaches 7.5% when above, scolder is too expanded, and causes the welding portion instability, and is very undesirable.
According to the welding thing, sometimes the impregnability of Ag scolder is compared its autgmentability and pay attention to more.For example, when the vacuum tube that requires vacuum tight and vacuum sphere and micro-element were welded, if the impregnability height, scolder can invade fine clearance, can improve welding reliability.Particularly in the welding of vacuum tube and micro-element, owing to there is no need to obtain intensity, so low Mn or the Ag scolder that do not have a Mn are particularly suitable for welding airtight member and micro-element by adding Mn.
The present invention 3 Ag solder for welding is formed by silver (Ag) by tin (Sn), the copper (Cu) of 2.5-10 weight %, the 2.5 weight % of 1.0-10.0 weight % following nickel (Ni), remainder.By adding the nickel (Ni) below the 2.5 weight %, can improve wetability or the autgmentability and the weld strength of soldering part.When Ni content surpasses 2.5%, cause liquidus temperature to raise, be difficult to the liquidus temperature of Ag scolder is controlled at below 900 ℃.
In these Ag scolders, can replace part or all tin with indium (In).Replace a part of Sn or whole Sn with In, also the solidus temperature of Ag scolder can be controlled at more than 800 ℃, liquidus temperature is controlled at below 900 ℃.The autgmentability of Ag scolder or the autgmentability of soldering part can be improved simultaneously, weldability can be improved like this.
When the Ag scolder contained manganese (Mn), also available titanium (Ti) was replaced part or all Mn.When replacing part or all branch Mn, can reach and above-mentioned same effect, that is, guarantee autgmentability and improve weld strength with Ti.Even soldered part has passive film to cover, still not needing to plate Ni just can soldering.
It is the matrix of principal component that above-mentioned any Ag scolder all exists with Ag that is ductile and Cu under solid state, so that surround the small compound of separating out that contains Sn.So can stop the be full of cracks that contains the Sn compound and the expansion of enbrittling, thereby the processability during improvement manufacturing Ag scolder (, forging, calendering, wire drawing).Simultaneously, after welding, protected the embrittlement of weld layer.
If the composition of above-mentioned Sn surpasses 10%, that separates out in Ag-Cu matrix contains the Sn compound and can increase greatly, causes the embrittlement of scolder self.Because solidus temperature excessively reduces, the cardinal principle standard of the Sn amount in the Sn compound of separating out under the solid state is 5%～60% (weight ratio).
Like this, Ag and Cu play a role jointly to the material property of whole scolder, particularly can left and right sides solidus temperature and liquidus temperature and mechanical strength.Meanwhile, the mechanical shock that is communicated to the welding position be can absorb after the welding, the generation and the propagation of be full of cracks suppressed.Since by Ag-Cu matrix surround separate out contain the Sn compound, so also have prevention to contain the effect that the Sn compound is the be full of cracks expansion of starting point.
In order to adjust solidus temperature and liquidus temperature, the ratio of Ag/ (Ag+Cu) is preferably 89.4～97.5%
Above-mentioned any Ag scolder, its manufacturing cost and former Ag scolder are roughly the same, even not using the Pd of high price is scolder (JIS, Z3267) and Au be scolder (JIS, Z3226), by being used in combination with existing Ag scolder, also can carry out the soldering of multistage substep, the manufacturing cost of end article is reduced.
Owing to suppressed to be welded the softening of member mother metal under the brazing operation temperature, so can guarantee the operating characteristic of end article.Because the melt temperature scope of Ag scolder of the present invention is 800～900 ℃, so the selecting range of other scolders is very wide in each section.The temperature of actual soldering weld job equates or is higher than this temperature with solidus temperature, be preferably under the temperature than the high tens of degree of liquidus temperature to carry out.
Owing to do not contain Pb, Zn, Cd etc. in forming,, so just do not need to use necessary flux (flux) and matting thereof in the atmospheric treatment so be suitable for soldering in vacuum chamber.And then, because have sufficient autgmentability and impregnability, so, even when the his-and-hers watches mask has stainless steel of passivity epithelium etc. to weld, the pre-treatment that does not also need to plate Ni.Because impregnability is good, be fit to air-tightness is had the welding of desired member and small electric subassembly.
Other features of the present invention and effect can be clearer and more definite after the detailed description of following specific embodiment of process and comparative example.
Description of drawings
Fig. 1 is expressed as used test film in the shear strength that confirms effect of the present invention and carry out and the impregnability test.
Fig. 2 is the key diagram that has used the multistage substep soldering of Ag scolder of the present invention.
Among the figure, 1 is soldered parts, and 2 is Ag scolder of the present invention, and 3 is stainless steel substrate, and 4 is aluminum oxide substrate, and 5 is the Cu parts, and 7 are existing scolder.
The best mode that carries out an invention
(the test making of Ag scolder)
Various composition blanks with diameter 50mm, length 400mm, about in a vacuum 1050 ℃ are carried out selecting 350～750 ℃ of annealing behind the vacuum melting, select the working modulus of 3-30% to roll, repeat necessary number of times, after being processed into 0.3mm thickness, as final processing, utilize cutting cutter to be processed into the tabular scolder of Rack (as 30mm), it is shown in table 1 and table 2 as test with scolder.
When needing wire rod, utilize extruding that above-mentioned blank is squeezed into diameter 10mm, with its annealing (350～750 ℃) and hot candied (working modulus 3-30%), repeat necessary number of times again, obtain the wire rod of diameter 0.1mm.
Table 1
| The embodiment comparative example | Form (weight %) | Remarks | ||||||||
| Mn | Ti | Sn[ | In] | Ni | Surplus portion | Reference | The material of soldered thing | |||
| (Cu) | (Ag) | (Ag+Cu) | Ag×100 | |||||||
| (Ag+Cu) | ||||||||||
| Embodiment 1 embodiment 2 embodiment 3 embodiment 4 comparative examples 1 embodiment 5 embodiment 6 | 0.1 0.3 2.5 6.0 7.5 1.5 1.5 | 0 0 0 0 0 0.5 2.0 | 4.0 4.0 4.0 4.0 4.0 4.0 4.0 | 0 0 0 0 0 0 0 | 0 0 0 0 0 0 0 | 6.0 6.0 6.0 6.0 6.0 6.0 6.0 | 89.9 89.5 87.5 85.0 82.5 88.0 86.5 | 95.9 95.5 93.5 91.0 88.5 94.0 92.5 | 93.7 93.7 93.6 93.4 93.2 93.6 93.5 | Do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS |
| Embodiment 7 embodiment 8 embodiment 9 embodiment 10 comparative examples 2 | 0.1 0.3 2.5 6.0 7.5 | 0 0 0 0 0 | 4.0 4.0 4.0 4.0 4.0 | 0 0 0 0 0 | 1.0 1.0 1.0 1.0 1.0 | 6.0 6.0 6.0 6.0 6.0 | 88.9 88.5 86.5 84.0 81.5 | 94.9 94.5 92.5 90.0 87.5 | 93.7 93.7 93.5 93.3 93.1 | Do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS |
| Comparative example 3 embodiment 11 embodiment 12 comparative examples 4 embodiment 13 embodiment 14 | 1.5 1.5 1.5 1.5 1.5 1.5 | 0 0 0 0 0 0 | 0.1 1.0 10.0 20.0 4.0 4.0 | 0 0 0 0 1.0 5.0 | 0 0 0 0 0 0 | 6.0 6.0 6.0 6.0 6.0 6.0 | 92.4 91.4 82.5 72.5 87.5 83.5 | 98.4 97.4 88.5 78.5 93.5 89.5 | 93.9 93.3 93.2 92.3 93.6 93.5 | Do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS |
| Embodiment 15 embodiment 16 comparative examples 5 | 1.5 1.5 1.5 | 0 0 0 | 4.0 4.0 4.0 | 0 0 0 | 0.1 2.0 5.0 | 6.0 6.0 6.0 | 88.4 86.5 83.5 | 94.4 92.5 89.5 | 93.6 93.5 93.3 | Nothing plating SUS and nothing plating SUS do not have the SUS of plating and do not have the SUS of plating and do not have plating SUS and do not have plating SUS |
| Comparative example 6 embodiment 17 embodiment 18 comparative examples 7 | 1.5 1.5 1.5 1.5 | 0 0 0 0 | 4.0 4.0 4.0 4.0 | 0 0 0 0 | 0 0 0 0 | 1.0 2.5 10.0 20.0 | 93.5 92.0 84.5 74.5 | 94.5 94.5 94.5 94.5 | 98.7 97.3 89.4 78.8 | Do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS |
| Embodiment 19 comparative examples 8 | 0.5 0.5 | 0 0 | 1.0 1.0 | 0 0 | 0 0 | 2.5 0.5 | 96.0 98.0 | 98.5 98.5 | 97.5 99.5 | Nothing plating SUS and nothing plating SUS do not have the SUS of plating and do not have the SUS of plating |
Table 2
| The embodiment comparative example | Form (weight %) | Remarks | ||||||||
| Mn | Ti | Sn[ | In] | Ni | Surplus portion | Reference | The material of soldered thing | |||
| (Cu) | (Ag) | (Ag+Cu) | Ag×100 | |||||||
| (Ag+Cu) | ||||||||||
| Embodiment 20 embodiment 21 embodiment 22 embodiment 23 | 0 0 0 0 | 0 0 0 0 | 1.0 4.0 7.0 10.0 | 0 0 0 0 | 0 0 0 0 | 6.0 6.0 6.0 6.0 | 93.0 90.0 87.0 84.0 | 99.0 96.0 93.0 90.0 | 93.9 93.7 93.6 93.3 | Do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS and do not have plating SUS |
| Embodiment 24 embodiment 25 embodiment 26 | 0 0 0 | 0 0 0 | 4.0 4.0 4.0 | 0 0 0 | 0.5 1.5 2.5 | 6.0 6.0 6.0 | 89.5 88.5 87.5 | 95.5 94.5 93.5 | 93.7 93.6 93.6 | Nothing plating SUS and nothing plating SUS do not have the SUS of plating and do not have the SUS of plating and do not have plating SUS and do not have plating SUS |
| Embodiment 27 embodiment 28 embodiment 29 | 2.5 2.5 2.5 | 0.5 0.5 0.5 | 1.0 1.0 1.0 | 0 0 0 | 0.1 0.1 0.1 | 6.0 6.0 6.0 | 89.9 89.9 89.9 | 95.1 95.1 95.1 | 94.5 94.5 94.5 | The Al2O3 that does not have plating SUS and 96% does not have plating SUS and Cu Cu and Cu |
(evaluation method, appreciation condition)
As shown in Figure 1, prepare the nothing plating corrosion resistant plate of 2 wide 24mm * long 125mm * thick 3mm, make the part at its both ends overlapping, 2～4mm roughly as shown in Figure 1 sandwiches the test formed shown in the table 1 with tabular scolder 2 at lap.According to the liquidus temperature of used scolder, after selection welding temperature (as 875～925 ℃) is carried out soldering, estimate weldability according to JIS-Z-3192 (shearing test method of soldering seam).The corrosion resistant plate of implementing plating Ni is in advance carried out same soldering welding as a reference.
Measure respectively composition test respectively with 1 of scolder) shear strength (N/mm
2), 2) autgmentability, 3) impregnability, and observe, be that benchmark carries out comprehensive assessment again with the observed result, it the results are shown in table 3 and table 4.The evaluation of shear strength is undertaken by following benchmark.
350N/mm
2When above: estimate A (good)
150～350N/mm
2The time: estimate B (well)
150N/mm
2When following: estimate C (bad)
The evaluation of autgmentability is carried on nothing plating SUS plate being die-cut into to test respectively forming of diameter 15mm with the scolder plate, and (expansion) situation that flows of scolder on the SUS plate surface was estimated by following benchmark when observation was heated to 875～925 ℃.
During heating more than the diameter 30mm of scolder area: estimate A (good)
The diameter of scolder area is 15～30mm during heating: estimate B (well)
There is not expansion (or diameter is less than 15mm): estimate C (bad)
The evaluation of impregnability shown in Fig. 1 (b), at about 0.05mm of 2 overlapping welding things 1 gap A point place, is placed the scolder of φ 1.0, fusion.Then, utilize the capillarity of motlten metal to observe the arrival degree that scolder is ordered to opposition side B, by following benchmark evaluation.
Arrive the B point fully: estimate A (good)
Almost arrive the B point: estimate B (well)
No show B point: estimate ℃ (bad)
Even the property sheared, autgmentability and impregnability all reach above-mentioned requirements, but temperature range is not in the target temperature range of scolder of the present invention, promptly can not satisfy solidus temperature more than 800 ℃, liquidus temperature causes that in the precondition below 900 ℃ the product of vacuum chamber pollution is also thought substandard product.
Table 3
| The embodiment comparative example | Shear strength (N/mm 2) | Autgmentability | Impregnability | The feature of remarks scolder or soldering part | Synthetic determination |
| Embodiment 1 embodiment 2 embodiment 3 embodiment 4 comparative examples 1 embodiment 5 embodiment 6 | B B A～B B B A～B B | C B B B B B B | A A A A A A A | Autgmentability is poor slightly, impregnability is fine, integral solder is good.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good.Cause goods and and stove internal contamination by Mn.Weld strength, impregnability, autgmentability all good welds intensity, impregnability, autgmentability are all good. | 0000 * 00 |
| Embodiment 7 embodiment 8 embodiment 9 embodiment 10 comparative examples 2 | B A～B A～B A～B B | C B B B B | A A A A A | Autgmentability is poor slightly, impregnability is fine, integral solder is good.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, expansion are all good.Weld strength, impregnability, autgmentability are all good.Cause goods and stove internal contamination by Mn. | 0000 * |
| Comparative example 3 embodiment 11 embodiment 12 comparative examples 4 embodiment 13 embodiment 14 | A B B C B B | B B A B B B | A A A A A A | It is all good to be difficult to that liquidus temperature (fusion end temp) is controlled at 900 ℃ of following weld strengths, impregnability, autgmentability.Weld strength, impregnability, autgmentability are all good.The Sn compound is huge, shears by force and reduces.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good. | * zero zero * 00 |
| Embodiment 15 embodiment 16 comparative examples 5 | B B B | A A B | A A A | Weld strength, impregnability, autgmentability are all good.Weld strength, to soak into the flight of steps leading to a palace hall, autgmentability all good.Solidus temperature and liquidus temperature all form high-temperatureization. | 00 * |
| Comparative example 6 embodiment 17 embodiment 18 comparative examples 7 | B B B B | A B B B | A A A A | Be unfavorable for solidus temperature is controlled at more than 800 ℃.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good.Be unfavorable for solidus temperature is controlled at more than 800 ℃. | * zero zero * |
| Embodiment 19 comparative examples 8 | A A | B C | A A | Weld strength, impregnability, autgmentability are all good.Liquidus temperature forms high temperatureization. | ○ × |
Table 4
| The embodiment comparative example | Shear strength (N/mm 2) | Autgmentability | Impregnability | The feature of remarks scolder or soldering part | Synthetic determination |
| Embodiment 20 embodiment 21 embodiment 22 embodiment 23 | B B B B | C C C C | A A A A | Autgmentability is poor slightly, impregnability is fine, integral solder is good.Autgmentability is poor slightly, impregnability is fine, integral solder is good.Autgmentability is poor slightly, impregnability is fine, integral solder is good.Autgmentability is poor slightly, impregnability is fine, integral solder is good. | 0000 |
| Embodiment 24 embodiment 25 embodiment 26 | B B A～B | B B B | A A A | Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good. | 000 |
| Embodiment 27 embodiment 28 embodiment 29 | B B A～B | B B A～B | A A A | Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good.Weld strength, impregnability, autgmentability are all good. | ○ ○ ○ |
Ag scolder embodiment and the comparative example formed shown in following his-and-hers watches 1 and the table 2 specify.
(embodiment 1～4)
Sn amount is set at 4.0%, changes the Mn amount by 0.1%, 0.3%, 2.5%, 5.0%, after carrying out soldering and handling, measure shear strength.Mn in [Ag-Cu-Mn-Sn] alloy amount is respectively 0.1%, 0.3%, 2.5% and 5.0% when any, and shear strength is 150～350N/mm
2, be evaluated as B, show good intensity
Each scolder lift-launch that is punched to diameter 15mm is not being plated on the SUS plate of Ni, autgmentability experiment when carrying out soldering and handle, Mn content is that 0.3%, 2.5%, 5.0% o'clock (embodiment 2～4) all present the expansion about 15～30mm, is evaluated as B, shows good autgmentability.On the other hand, Mn content is 0.1% o'clock (embodiment 1), and expanding area is evaluated as C less than 15mm.
In the impregnability test, Mn content is selected from 0.1%, 0.3%, 2.5% and 5.0%, and scolder all is impregnated in the fine clearance of 2 overlapping corrosion resistant plates, reaches an opposite side fully, is evaluated as A, presents good welding quality.
Mn content is 0.1% o'clock, and autgmentability is poorer slightly, but owing to have sufficient impregnability, good as the weldability of scolder in actual applications.Vacuum tube is being sealed when welding with the small electric subassembly, the impregnability of scolder becomes prior key element, and the scolder of embodiment 1 is specially adapted to the purposes of small soldering and vacuum tight.
The solidus of any scolder of embodiment 1-4 (fusion begins) temperature is all more than 800 ℃, and liquidus temperature all below 900 ℃, reaches target temperature range.
Though do not illustrate in table 1 and 2, but the Ag scolder of composition that has used embodiment 1-4 is as soldered construction material, when selecting to implement the SUS plate of plating Ni, present more stable shear strength (roughly improving 10～50%) and good impregnability, even autgmentability, expanding area has approximately all improved 10-30% among the embodiment 1-4.
(comparative example 1)
As a comparative example, make Sn content and be 4.0%, Mn content is [Ag-Cu-Mn-Sn] blank of 7.5%, and be made into the thick tabular scolder of 0.1mm.Should tabular solder clip do not have between the plating SUS plates, after carrying out soldering and handling, measure shear strength equally at 2 shown in Figure 1.Obtain 150～350N/mm
2Shear strength, be evaluated as B, show good intensity.
Below, comparative example 1 (the Mn amount the is 7.5%) scolder that is die-cut into diameter 15mm is carried not having on the plating SUS plate, carry out soldering and handle, according to this autgmentability experiment, demonstrate the autgmentability (estimating B) of 15～30mm, intensity, autgmentability are all good.Impregnability is also good, and integral solder is better.Yet along with Mn content increases, the evaporation capacity of the Mn that vapour pressure is higher increases, and produce the problem of polluting welding thing and furnace inner environment, and then according to the soldering condition, the Ag scolder is expanded too, and welding stability is not good enough sometimes.Scolder quality when making scolder also produces deviation, has the not good enough problem of quality stability.
By these embodiment and comparative example, the Mn amount presents good weldability in 0.1～6% scope as can be known.
(embodiment 5,6)
In embodiment 1-4 and comparative example 1,, when the Ti of Mn and ormal weight coexists, also can give play to equal effect though present the effect of adding Mn.In embodiment 5 and 6, obtaining Mn amount is 1.5%, and Ti makes 0.1 thick tabular scolder after being respectively the blank of 0.5% and 2.0% [Ag-Cu-Mn-Sn-Ti].These tabular solder clip are not had between the plating SUS plates at 2 shown in Figure 1, after carrying out soldering and handling, measure shear strength equally.When containing 0.5%Ti, demonstrate 350N/mm
2Above shear strength (estimating A) and 150～350N/mm
2Shear strength (estimate B), when containing 2.0%Ti, demonstrate 150～350N/mm
2Shear strength (estimate B), show good intensity.
The various scolders that are die-cut into diameter 15mm are carried not having on the plating SUS plate,, on these two kinds of scolders, demonstrate the expansion (estimating B) of 15～30mm, manifested good autgmentability according to the autgmentability experiment of carrying out the soldering processing simultaneously.Utilize the observed result of impregnability of capillarity also very good.
As a reference, Mn amount is similarly 1.5%, the Ti amount increased by 5% o'clock, generates a large amount of CuTi compounds, causes processability to reduce, and the operation of machining plate-like and the wire complexity that becomes is unfavorable for commercial Application as can be known.
(embodiment 7～10 and comparative example 2)
In [Ag-Cu-Mn-Sn] of embodiment 1-6 and comparative example 1 alloy, Mn amount is 0.1%～6.0% or its part when being replaced as Ti, has given play to good weld strength (shear strength) and autgmentability.Embodiment 7～10th, and the situation of the Ni of interpolation 1.0% is assessed its shear strength and autgmentability in the alloy of embodiment 1～4.The results are shown in table 3, shear strength improve 10-40% (estimate A～B), autgmentability (wetability) is also further stable.Though contain Mn or Ti, impregnability is very good.
On the other hand, as a comparative example 2, the Mn amount is 7.5% o'clock, and the same with comparative example 1, the shear strength after the soldering, autgmentability, impregnability have all reached qualified benchmark, and still, the evaporation capacity of Mn increases, and confirms to produce pollution in the stove, and is undesirable.
(embodiment 11～12 and comparative example 3～4)
In [Ag-Cu-Mn-Sn] alloy of embodiment 1-10 and comparative example 1,2, it is 4.0% o'clock that Sn is measured, and all presents shear strength, autgmentability, impregnability, but in embodiment 11 and 12, Sn amount becomes 1.0% and respectively at 10% o'clock, confirms also to have brought into play good welding effect.That is, manufacturing Sn amount is 1.0% and 10% scolder, and these tabular solder clip are not had between the plating SUS plates at 2 shown in Figure 1, carries out soldering and handles.Afterwards, measure shear strength, the Sn amount is 1.0%, 10% o'clock, all presents 150～350N/mm
2Shear strength (estimate B), given play to good intensity.The various scolders that are die-cut into diameter 15mm are carried not having on the plating SUS plate, carry out soldering simultaneously and handle, according to this autgmentability experiment, the Sn amount is 1.0% o'clock (embodiment 9), demonstrates the expansion (estimating B) of 15～30mm, has given play to good autgmentability.The Sn amount is 10% o'clock (embodiment 10), demonstrates the above expansion of 30mm (estimating A), has further improved autgmentability, no matter how the Sn amount changes, impregnability is best.
By between 1.0%～10%, adjusting the content of Sn, can keep the good welds of Ag scolder, solidus temperature, liquidus temperature can be controlled at again simultaneously in 800～900 ℃ the target zone.
Opposite with it, in comparative example 3 Sn being measured is 0.1% o'clock, and shear strength is at 350N/mm
2More than (estimate A), expanding area be 15～30mm (estimating B), every specific character is all fine.Yet the liquidus temperature of Ag scolder is failed below 900 ℃, owing to do not reach the 1st purpose of the present invention, so undesirable.As a comparative example 6, it is 20% o'clock that Sn is measured, according to the autgmentability experiment, demonstrate 15mm above～expansion (estimating B) of 30mm, though also in acceptability limit, the measurement result of shear strength is lower than 150N/mm
2(estimate C), weld strength is inferior as can be known.Think that according to microscopical fabric study its reason is to have generated a large amount of Sn compounds.
(embodiment 13～14)
In embodiment 11～12 and comparative example 3～4, though show the proper range of Sn amount, the In coexistence of Sn and ormal weight also can obtain equal effect.In embodiment 13 and 14, it is 4% that Sn is measured, and In amount is taken as 1.0% and 5.0% respectively, obtain [Ag-Cu-Mn-Sn-In] blank after, make 0.1 thick tabular scolder.So tabular solder clip is not had between the plating SUS plates at 2 shown in Figure 1, after carrying out soldering and handling, measure shear strength equally.Embodiment 13 and 14 demonstrates 150～350N/mm
2Shear strength (estimate B), given play to good intensity.Each scolder that is die-cut into diameter 15mm is carried not having on the plating SUS plate, carries out soldering simultaneously and handle, according to the autgmentability experiment, do not have demonstrate on the plating SUS plate more than the 15mm～expansion (estimating B) of 30mm, show good autgmentability.
Though do not illustrate in the table, as a reference, Sn amount is remained on 4.0% and the In amount is increased at 10% o'clock, processability significantly reduces, and is processed into tabular as can be known and operation wire becomes very complicated, and is can not industry practical.
(embodiment 15～16 and comparative example 5)
In embodiment 7～10 and comparative example 2, show that the Ni in [Ag-Cu-Mn-Sn-Ni] alloy is measured is at 1.0% o'clock, be suitable for the Mn amount of shear strength, autgmentability.In embodiment 15 and 16, it is 4.0% that Sn is measured, Mn is measured is 1.5%, change the Ni amount, confirms its effect.That is, Ni amount is taken as 0.1% (implementing 13) and 2.5% (embodiment 14) respectively, obtain [Ag-Cu-Mn-Sn-Ni] blank after, produce the thick tabular scolder of 0.1mm.These tabular solder clip are not had between the plating SUS plates at 2 shown in Figure 1, after carrying out soldering and handling, measure shear strength equally.Any one embodiment demonstrates 150～350N/mm
2Shear strength (estimate B), given play to good intensity.The various scolders lift-launchs that are die-cut into diameter 15mm are not being had on the plating SUS plate, carrying out the autgmentability experiment that soldering is handled simultaneously, both sides demonstrate the expansion (estimating A) more than the 30mm on nothing plating SUS plate, given play to good autgmentability.Utilize extruder that above-mentioned stock is squeezed into diameter 10mm, with its annealing (350～750 ℃) and hot candied (working modulus 3～30%), repeat necessary number of times, obtain the wire rod of diameter 0.1mm, the same shear strength of measuring is implemented the autgmentability evaluation, in equal Ni weight range, given play to good characteristic, impregnability is also fine.
On the other hand, as a comparative example 5, the Ni amount is increased to 5.0%, to carry out same soldering and handle, the shear strength after the welding is 150～350N/mm
2(estimate B) according to the autgmentability experiment, is die-cut into the scolder of diameter 15mm, do not have demonstrate on the plating SUS plate more than the 15mm～expansion (estimating B) of 30mm, impregnability are also fine.Yet liquidus temperature raises, owing to can not be controlled at below 900 ℃, so very undesirable.
As mentioned above, the Ni amount in the scolder possess weld strength (shear strength), autgmentability and impregnability simultaneously, and liquidus temperature can be controlled at below 900 ℃ also below 2.5%.
(embodiment 17～18 and comparative example 6～7)
In embodiment 17,18, the suitable Cu amount of conclusive evidence in [Ag-Cu-Mn-Sn] alloy or [Ag-Cu-Mn-Sn-Ni] alloy.The content of contained Cu amount and Ag all is adjusted within the setting scope the solidus temperature of alloy and liquidus temperature and plays an important role in the Ag scolder.
In embodiment 17, it is 2.5% (the Mn amount is 1.5%, and Sn is 4.0%) that Cu is measured, Ag is measured is 92.0% (Ag+Cu=94.5%, Ag/ (Ag+Cu)=97.4%).After carrying out the soldering processing, the shear strength that demonstrates is 150～350N/mm
2(estimate B), 15mm be above～and the expansion (estimating B) of 30mm, scolder be impregnated into a relative side fully, all demonstrate good characteristic in the gap of welding thing.And then, also solidus temperature, the liquidus temperature of scolder can be controlled in 800～900 ℃ the scope.
In embodiment 18, Cu is measured is 10.0%, when Ag is measured and is 84.5% (Ag+Cu=94.5%, Ag/ (Ag+Cu)=89.4%), and after carrying out soldering and handling, shear strength is 150～350N/mm
2(estimating B).Demonstrate in the autgmentability test 15mm above～expansion of 30mm, impregnability is also fine, in this is formed, all demonstrates good characteristic, solidus temperature, liquidus temperature also can be controlled in 800～900 ℃ the scope.
Opposite with it, as a comparative example 6, prepare the Ag scolder of Cu amount 1.0%, Ag amount 93.5% (Ag+Cu=94.5%, Ag/ (Ag+Cu)=98.9%), after carrying out soldering and handling, shear strength is 150～350N/mm
2(estimating B), in the autgmentability experiment, the scolder that is die-cut into diameter 15mm demonstrates autgmentability fabulous more than the 30mm (estimating A) on nothing plating SUS plate, and two specific characters are all fine.Impregnability is also fabulous.Yet this composition can not be controlled at liquidus temperature below 900 ℃.
As a comparative example 7, Cu is measured is 20.0%, when Ag is taken as 74.5% (Ag+Cu=94.5%, Ag/ (Ag+Cu)=78.8%), and after carrying out soldering and handling, shear strength is 150～350N/mm
2(estimating B) given play to good intensity, in the autgmentability experiment, do not having the expansion (estimating B) that presents 15～30mm on the plating SUS plate.Impregnability is also best.Yet solidus temperature is difficult to be controlled at more than 800 ℃.
(embodiment 19 and comparative example 8)
In embodiment 19, Cu measured be 2.5% (the Mn amount is 0.5%, Sn amount be 1.0%), the Ag amount is increased to 96.0% (Ag+Cu=98.5%, Ag/ (Ag+Cu)=97.5%), after carrying out soldering and handle with this composition, shear strength is at 350N/mm
2More than (estimate A), the expansion (estimating B) of autgmentability demonstrates 15mm above～30mm, impregnability is also fabulous.Solidus temperature and liquidus temperature can be controlled at 800～900 ℃ scope.
Opposite with it, in comparative example 8, it is that 0.5% (the Mn amount is 0.5%, and the Sn amount is 1.0%), Ag amount are 98.0% (Ag+Cu=98.5%, Ag/ (Ag+Cu)=99.5%) that Cu is measured.After carrying out the soldering processing, shear strength is at 350N/mm
2More than (estimate A), impregnability is also fabulous, but autgmentability (is estimated C) below 15mm.And liquidus temperature rises to 900 ℃, and is very undesirable.
(embodiment 20～23)
In embodiment 20～23, the Cu content of Ag scolder is taken as 6.0%, Sn content is taken as 1.0%, 4.0%, 7.0%, 10.0% respectively, and remainder is Ag, measures its weldability.In these are formed, owing to do not contain Mn, so in the mensuration of autgmentability, be lower than 15mm, inferior slightly, it is also fine that shear strength is evaluated as B, impregnability, and the overall merit of scolder weldability is fine, satisfied solidus temperature more than 800 ℃, liquidus temperature is in the target zone below 900 ℃.The Ag scolder of these compositions is compared with the autgmentability on single plane, when more paying attention to the impregnability to 2 welding thing gaps, for example, requires the welding of micro-member and when not wishing to contain the air-tightness such as vacuum tube of evaporated metal element, and is the most suitable.
(embodiment 24～26)
In embodiment 24～26, with Sn content be taken as 4.0%, Cu content is taken as 6.0%, Ni content is taken as 0.5%, 1.5%, 2.5% respectively, remainder is Ag, measures its weldability.In these were formed, shear strength, autgmentability, impregnability all demonstrated good characteristic, and weldability is fabulous as can be known.
(embodiment 27～29)
In embodiment 27～29, confirm that Ag scolder of the present invention is not limited to SUS, applicable to construction material widely.That is, up to embodiment 26, as the welding thing, the SUS (stainless steel) that has only selected not have the enforcement plating is as example, but in embodiment 27～29, thing selects not have plating SUS respectively and aluminium oxide, nothing are plated SUS and Cu, Cu and Cu as welding.Any situation all demonstrates good shear strength, autgmentability and impregnability.Though not shown in the table, when using plating SUS to replace not having plating SUS, present more stable shear strength, autgmentability and impregnability.
Below to Ag scolder of the present invention and existing Ag scolder are made up, the substep soldering of welding different parts successively describes.
For example, as shown in Figure 2, investigation welding fusing point on stainless steel substrate 3 is 1083 ℃ Cu parts 5, covers the situation of any materials members 4 such as welding ceramics, aluminium oxide on these Cu parts 5, at this moment, can not weld Cu parts 5 and following stainless steel substrate 3 and top member 4 simultaneously.When the solder side of Cu parts 5 upwards welded, scolder can be wandered, and can pollute Cu parts 5, and then the stainless steel substrate 3 below polluting.
Therefore, the solder side of Cu parts 5 is usually downward, at first welds a face, then another side is welded in 5 upsets of Cu parts again.
In example shown in Figure 2, when having the stainless steel substrate 3 of passivity tunicle and Cu parts 5, uses face of weld Ag scolder 2 of the present invention.At stainless steel substrate 3 with between the Cu parts 5 of assigned position configuration, insert the Ag solder sheet of the present invention of well cutting, atmosphere gas is heated to 920～925 ℃ carries out soldering.Because processing temperature is set at this scope, so can avoid the mother metal of Cu parts 5 is softened the generation harmful effect.Because Ag scolder autgmentability of the present invention is fabulous, do not handle so do not need that before welding stainless steel substrate 3 is made plating Ni
Below use the melt temperature existing Ag scolder 7 lower than the solidus temperature of Ag scolder of the present invention, other faces at the Cu parts for example weld aluminum oxide substrate 4.At this moment, make the solder side of Cu parts 5 downward, make again the assembly that is welded in advance on the stainless steel substrate 3 reverse to, like this, under the processing temperature below 800 ℃, all components heat treated is carried out soldering.
Above-mentioned soldering is handled and can be carried out in atmosphere, also can carry out in vacuum chamber.
Following effect of carrying out the substep soldering according to embodiment 30～33 confirmation uses Ag scolder of the present invention.
(embodiment 30)
Utilize Ag scolder of the present invention to weld the 1st welding position in advance, then dispose known eutectic Ag scolder [all the other are Cu 72%Ag-] (780 ℃ of solidus temperatures in the 2nd welding position, 780 ℃ of liquidus temperatures), be chosen in the temperature of above-mentioned the 1st welding position not fusion of used Ag scolder of the present invention, carry out heat treated simultaneously with the 1st welding position.After welding is finished, the 1st welding position is carried out the evaluation of shear strength, impregnability, autgmentability, impregnability is evaluated as A, and shear strength and autgmentability are evaluated as A～B.
(embodiment 31)
Utilize BNi-2 (995 ℃ of solidus temperatures, 1000 ℃ of liquidus temperatures) welding the 1st welding position of existing scolder JIS Z3265.Then, weld the 2nd welding position with Ag scolder of the present invention.And then, dispose known eutectic Ag scolder (780 ℃ of solidus temperatures, 780 ℃ of liquidus temperatures) in the 3rd welding position.Above-mentioned the 2nd welding position with the solidus temperature of Ag scolder of the present invention and the 3rd welding position with the temperature between the liquidus temperature of eutectic Ag scolder under, the 1st welding position and the 2nd welding position are carried out heat treated simultaneously, finish the soldering of multistage substep.Subsequently, impregnability, shear strength and autgmentability are estimated in the 2nd welding position.Impregnability is evaluated as A, and shear strength and autgmentability are evaluated as A～B.
(variation)
In embodiment 30～31, soldered owner does not have the plating corrosion resistant plate, but promptly is used in the stainless welding of having carried out plating Ni in advance, can both obtain good result aspect shear strength, impregnability and the autgmentability yet.As shown in Figure 2, even when a side or two sides are other metals, alloys such as Cu, or be aluminium oxide etc. when nonmetal, all obtained good shear strength, impregnability and autgmentability in the welding position.
The invention provides a kind of unprecedented Ag scolder with 800～900 ℃ of solidus temperatures and liquidus temperature.Owing to do not use the Pd of high price, so can low cost weld.
During as a kind of scolder in the soldering of multistage substep, the range of choice of the selecting range of another kind of scolder and weld job temperature is all very big with Ag scolder of the present invention.
In embodiment 27～29, confirm that Ag scolder of the present invention is not limited in and be used for SUS that it can be applicable to more material members.That is, in embodiment 26, the SUS (stainless steel) that has only selected not implement to electroplate as soldered thing is as example, but in embodiment 27～29, selected not have plating SUS and aluminium oxide, nothing plating SUS and Cu, Cu and Cu respectively as the welding thing.Any situation all demonstrates good shear strength, autgmentability and impregnability.Though not shown in the table, with plating SUS the time, present more stable shear strength, autgmentability and impregnability.
Particularly in the multistage substep soldering when welding causes the softening parts of mother metal easily, can use effectively.
No matter the material of soldered thing how, Ag scolder of the present invention can be extensive use of, even at surperficial unreal plating Ni such as stainless steels, still can obtain good soldering effect.
Ag material of the present invention is not only applicable to the processing in the atmosphere, is applicable to the soldering in vacuum chamber yet, and does not need the FLUX solvent to handle.
Claims (1)
1. an Ag solder for welding is characterized in that, its solidus temperature is more than 800 ℃, and liquidus temperature is below 900 ℃, and it is by the tin of 1.0～4.0 weight %, the copper of 2.5～10 weight %, the nickel below the 2.5 weight %, and remainder is formed by silver.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001087623 | 2001-03-26 | ||
| JP087623/01 | 2001-03-26 | ||
| JP087623/2001 | 2001-03-26 | ||
| JP390150/01 | 2001-12-21 | ||
| JP2001390150A JP2002361478A (en) | 2001-03-26 | 2001-12-21 | Ag BRAZING FILLER METAL FOR JOINING AND BRAZING METHOD USING THE SAME |
| JP390150/2001 | 2001-12-21 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1377753A CN1377753A (en) | 2002-11-06 |
| CN1196563C true CN1196563C (en) | 2005-04-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02106267 Expired - Fee Related CN1196563C (en) | 2001-03-26 | 2002-03-07 | Ag solder for welding and soldering method using it |
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| JP (1) | JP2002361478A (en) |
| CN (1) | CN1196563C (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4643149B2 (en) * | 2004-01-26 | 2011-03-02 | 芝府エンジニアリング株式会社 | Brazing material |
| CN100457370C (en) * | 2006-08-17 | 2009-02-04 | 贵研铂业股份有限公司 | Silver-based alloy solder and application thereof in vacuum circuit breaker step soldering |
| CN100439029C (en) * | 2006-08-18 | 2008-12-03 | 贵研铂业股份有限公司 | Silver-based alloy solder and application thereof in vacuum circuit breaker step soldering |
| JP2009113089A (en) * | 2007-11-07 | 2009-05-28 | Toshiba Corp | Joining material for vacuum valve |
| JP2009283313A (en) * | 2008-05-22 | 2009-12-03 | Toshiba Corp | Joining material for vacuum bulb |
| CN102328157A (en) * | 2011-09-09 | 2012-01-25 | 合肥工业大学 | Method for manufacturing SnAgCu lead-free solder |
| CN103406684B (en) * | 2013-08-01 | 2016-01-06 | 中国航空工业集团公司北京航空材料研究院 | A kind of silver-copper-indium-nickel middle temperature brazing material |
| CN108340094B (en) * | 2017-01-23 | 2020-11-17 | 北京有色金属与稀土应用研究所 | Ag-Cu-In-Sn-Ti alloy solder and preparation method and application thereof |
| CN107214437A (en) * | 2017-07-31 | 2017-09-29 | 安徽华众焊业有限公司 | It is a kind of without silver-base solder of the indium without cadmium |
| CN107234369A (en) * | 2017-07-31 | 2017-10-10 | 安徽华众焊业有限公司 | A kind of high temperature is without copper silver-base solder |
| CN112605556A (en) * | 2020-12-22 | 2021-04-06 | 无锡日月合金材料有限公司 | Brazing filler metal for multistage brazing of vacuum device and preparation method thereof |
-
2001
- 2001-12-21 JP JP2001390150A patent/JP2002361478A/en active Pending
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| JP2002361478A (en) | 2002-12-18 |
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