CN104889594A - Low-temperature ultrasonic SnBi-based brazing filter metal, production method thereof and method for ultrasonically brazing ceramics and/or ceramic-based composite - Google Patents
Low-temperature ultrasonic SnBi-based brazing filter metal, production method thereof and method for ultrasonically brazing ceramics and/or ceramic-based composite Download PDFInfo
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- CN104889594A CN104889594A CN201510306294.5A CN201510306294A CN104889594A CN 104889594 A CN104889594 A CN 104889594A CN 201510306294 A CN201510306294 A CN 201510306294A CN 104889594 A CN104889594 A CN 104889594A
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- base solder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/264—Bi as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/001—Joining burned ceramic articles with other burned ceramic articles or other articles by heating directly with other burned ceramic articles
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Abstract
The invention relates to low-temperature ultrasonic SnBi-based brazing filter metal, a production method thereof and a method for ultrasonically brazing ceramics and/or ceramic-based composite, belongs to the technical field of ceramic and ceramic-based composite brazing, and solve the problems that brazing can only be performed under high temperature, effective connection is hard to form, and residual heat stress formed during cooling causes weld cracking in the prior art are solved. The low-temperature ultrasonic SnBi-based brazing filter metal comprises Bi, Cu, Al, mixed rare earth (RE) and Sn. The production method includes: heating a muffle furnace, feeding Ar gas into the muffle furnace, placing a crucible with Cu into the muffle furnace until Cu melts completely, sequentially adding Al, Sn, Bi and mixed rare earth, and preserving heat for 20-60 minutes. The brazing method includes: applying pressure, using an ultrasonic tool head to directly press a to-be-welded part in a clamp, heating to 170-200 DEG C under an atmosphere environment, and applying ultrasonic brazing. The method uses ultrasonic brazing to connect ceramics and or ceramic composite.
Description
Technical field
The invention belongs to the soldering tech field of structural ceramics and composite thereof, be specifically related to a kind of low temperature ultrasonic SnBi base solder and preparation method thereof, and the method for ultrasonic brazing pottery and/or ceramic matric composite.
Background technology
The mechanical strength of pottery is high, have good wearability, corrosion resistance, and thermal stability is good.Sapphire is one the most frequently used in pottery.
Sapphire, due to its good optical property, is widely used in optics and window material.But along with contemporary optics system is to the demand of high-aperture optical material, the sapphire size obtained by Artificial Growth can not be satisfied the demands.At present, the unique channel of large scale optical window is acquired exactly by being connected together by fritter sapphire.Therefore, sapphire interconnection technique has become the focus of academia's words, has important research and practical value.
Connect sapphire by bonded process and there is certain integrity problem because the macromolecule in joint at high temperature easily decomposes, and bonding strength is not high.There is the defects such as hole in the weld seam that reaction sintering obtains, become the source, crack in sapphire fracture process.Soldering realizes ceramic material to connect the most frequently used method, the sapphire active solder of the soldering mainly Ag-Cu-Ti solder of current extensive use.By active element Ti and sapphire reaction, promote liquid solder and sapphire wetting combination.Whole welding process needs could realize connecting in vacuum environment and 850 DEG C of high temperature, from the process of high temperature (850 DEG C) cool to room temperature, because solder differs larger with sapphire thermal coefficient of expansion, cause welding point to leave very large residual stress, become the main cause of Joint Cracking.
Summary of the invention
The present invention will solve the existing active solder ceramic soldering of application and/or ceramic matric composite can only soldering under high temperature (850 DEG C), and is difficult to form the problem causing weld cracking in effective connection, cooling procedure due to residual thermal stress; And provide low temperature ultrasonic SnBi base solder and preparation method thereof, and the method for ultrasonic brazing pottery and/or ceramic matric composite.
For solving the problems of the technologies described above, in the present invention, the chemical composition of low temperature ultrasonic SnBi base solder is by weight percentage: 41.5 ~ 52.5%Bi, 0.05 ~ 0.15%Cu, 0.01 ~ 0.1%Al, 0.01 ~ 0.05% mishmetal, and surplus is Sn; Described mishmetal is that Pr forms by 50% ~ 70%Ce, 20% ~ 30%La, 10 ~ 15%Nd and surplus by weight percentage; Its preparation method carries out in the steps below: put into by Cu in crucible, Muffle furnace is heated to 1200 DEG C, and fills Ar gas wherein, crucible is put in Muffle furnace, insulation, until Cu melts completely, in succession adds Al, Sn, Bi and mixed rare earth, is then incubated 20 ~ 60 minutes; Low temperature ultrasonic SnBi base solder is obtained after cooling.
The method of low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or ceramic matric composite is carried out in the steps below:
Step one, get two pieces of potteries or one piece of pottery and one block of ceramic matric composite or two blocks of ceramic matric composites as to-be-welded pieces, be placed in acetone ultrasonic cleaning;
Step 2, by low temperature ultrasonic SnBi base solder compressing tablet according to claim 1, the thickness of sheet is 0.3 ~ 0.5mm, is cut into the size corresponding with to-be-welded pieces, obtains solder sheet;
Step 3, solder sheet folder and step one in step 2 are processed rear to-be-welded pieces surface to be welded between obtain treating weldment, then will treat that weldment is put into jig and clamped;
Step 4, apply the pressure of 0.2 ~ 1Mpa, be directly pressed in by Ultrasonic probe and treat on weldment in step 3 jig, under atmospheric environment, be heated to 170 ~ 200 DEG C, applying amplitude is that the ultrasonic wave of 5 μm carries out ultrasonic wave added soldering 50 ~ 1000s.
The present invention adopts using Al element as active element SnBi base solder, achieve (170 ~ 200 DEG C) ultrasonic brazing at a lower temperature and connect pottery (sapphire) and containing ceramic matric composite etc., containing the composite of ceramic base as the glass containing ceramic particle, silicon, aluminium alloy, magnesium alloy, titanium alloy etc.Present invention, avoiding the cracking of joint, achieve effective connection of pottery and/or ceramic matric composite, particularly sapphire welding.
The invention has the advantages that compared to existing technology:
1, the present invention take Al as the active element of ceramic soldering and/or ceramic matric composite, generates Al by Al to pottery and/or ceramic matric composite diffusion into the surface reaction
2o
3excessive layer, realizes pottery and/or ceramic matric composite substrate is connected with the effective of solder.
2, in the present invention, the content of Al is the fusing point of micro content (0.01%-0.1%), Al is 660 DEG C, and trace of Al can avoid the fusing point of Sn base solder significantly to rise, and avoids the Cu in Al and solder to react simultaneously and generates CuAl
2, CuAl and Cu
2the brittle intermetallic things such as Al, thus weaken weld seam.
3, in the present invention, Cu element can form Cu with the Sn element in solder
6sn
5, the Cu of generation
6sn
5as nucleating agent, increase the nucleation rate of SnBi eutectic structure, facilitate the refinement of β-Sn phase and rich Bi phase crystal grain, improve the fragility of solder.The elongation of solder never adds 21% of Cu element and has brought up to 39%.
4, the Cu element added in the present invention in weld seam forming process, the Cu of generation
6sn
5, thus crystal grain thinning.In seam organization, the refinement of crystal grain can improve toughness, reduces residual stress, thus the intensity of weld seam is promoted to some extent.
5, the present invention achieves low-temperature welding containing low temperature ultrasonic SnBi base solder, reduces the residual stress produced because the thermal coefficient of expansion of structural ceramics and solder does not mate in cooling procedure, thus greatly strengthens structural ceramics weldment reliability in use.And existing active solder (Ag-Cu-Ti solder) is in the welding of active element with Ti, because brazing temperature is higher, cause welding point residual stress in cooling procedure comparatively large, in use there is the problem of certain reliability.
6, low temperature ultrasonic SnBi base solder ultrasonic brazing pottery of the present invention and/or ceramic matric composite just can realize effectively connecting in atmospheric environment.And existing active solder (Ag-Cu-Ti solder) ceramic soldering and/or ceramic matric composite need to carry out in a vacuum furnace, harsher to the requirement of welding surroundings.
7, Ti's is expensive, and the less expensive of Al, the present invention uses Al to reduce the cost producing solder as active element.
8, Al can be significantly improved at Al adding of mixed rare earth
2o
3surface wetting, thus make can better be combined between Al with pottery or ceramic particle, adding of mixed rare earth can the tissue of refinement Sn base solder simultaneously.
Accompanying drawing explanation
Fig. 1 is ultrasonic wave added soldering sapphire schematic diagram; Fig. 2 is the DSC curve of low temperature ultrasonic SnBi base solder; Fig. 3 is the micro-organization chart of brazing filler metal alloy; Fig. 4 is the golden micro-organization chart that low temperature ultrasonic SnBi base solder closes; Fig. 5 is welding joint structure pattern; Fig. 6 is the change of welding point shear strength with ultrasonic amplitude; Fig. 7 is the impact that mishmetal adds Welded Joints shear strength; Fig. 8 is the nanometer Al of sapphire/solder Interface debond
2o
3particle SEM image; Fig. 9 is active element Al and Al
2o
3interracial contact atomic arrangement schematic diagram; Figure 10 is active element Al and Al
2o
3reaction epitaxial growth Al
2o
3thin layer schematic diagram; Wherein 1 in Fig. 1---upper sapphire to be welded, 2---lower sapphire to be welded, 3---solder, 4---Ultrasonic probe, 5---heater coil, 6---fixed mould, 7---variable-sized fixture.
Detailed description of the invention
Detailed description of the invention one: the chemical group prejudice table 1 of low temperature ultrasonic SnBi base solder in present embodiment:
Table 1 is the chemical composition (by weight percentage) of low temperature ultrasonic SnBi base solder
Wherein, the chemical group prejudice table 2 of minipool rare earth (RE):
Table 2 is the chemical composition (by weight percentage) of mishmetal (RE)
In present embodiment, the preparation method of low temperature ultrasonic SnBi base solder is as follows:
Put into by Cu in crucible, Muffle furnace is heated to 1200 DEG C, and fill Ar gas wherein, put into by crucible in Muffle furnace, insulation, until Cu melts completely, adds Al, Sn, Bi and mixed rare earth in succession, is then incubated 30 minutes; Low temperature ultrasonic SnBi base solder is obtained after cooling.
In present embodiment, low temperature ultrasonic SnBi base solder ultrasonic brazing sapphire method carries out in the steps below:
Step one, sapphire to be welded is placed in acetone ultrasonic cleaning 10min;
Step 2, low temperature ultrasonic SnBi base solder by mill milling, or rotate to get rid of in band carry out compressing tablet by getting rid of band machine, measure pricker material thickness, until pricker material thickness is 0.5mm, and be cut into the size of 10cm × 10cm with spiral micrometer;
Step 3, solder sheet folder and step one in step 2 are processed after two pieces of sapphire surfaces to be welded between form and treat weldment, then will treat that weldment is put into jig and clamped;
Step 4, applying 0.2Mpa pressure, be directly pressed on the sapphire weldment in step 3 jig, under atmospheric environment by Ultrasonic probe, be heated to 170 DEG C, setting ultrasonic amplitude is 5 μm, and ultrasonic wave application time is 50s, carry out ultrasonic wave added soldering, as shown in Figure 1.
Carry out Measurement accuracy to the low temperature ultrasonic SnBi base solder liquidus temperature of present embodiment, carry out heating differential analysis, result as shown in Figure 2.Learnt by curve, solder solidus 143.8 DEG C, liquidus curve 155.8 DEG C.Usually, brazing temperature is more than liquidus temperature tens degree.So brazing temperature is set as 170 DEG C, solder can soldering sapphire at low temperatures.
The microstructure SEM figure of low temperature ultrasonic SnBi base solder liquid alloy as shown in Figure 3.Wherein, grey form and aspect are the rich Bi phase of rich Bi phase and secondary precipitation, and light is β-Sn phase.Rich Bi phase crystal grain and thick can be observed from SEM figure, result in this brazing filler metal alloy fragility very big.And when adding of micro Cu in solder is fashionable, the rich Bi phase in solder obtains refinement, as shown in the SEM figure of Fig. 4.This be Cu owing to adding can and Sn reaction generation Cu
6sn
5.That first weld seam separates out in process of setting is high temperature Cu
6sn
5phase (fusing point 415 DEG C), Cu
6sn
5play the effect of nucleating agent, increase the nucleation rate of SnBi eutectic structure, thus facilitate the refinement of β-Sn phase and rich Bi phase.And the refinement of β-Sn phase and rich Bi phase adds the ductility of solder.
After ultrasonic brazing, the tissue topography of joint as shown in Figure 5.Adopt low temperature ultrasonic SnBi base solder to carry out ultrasonic brazing, postwelding, solder is combined closely with sapphire substrates, does not have obvious weld defect.Visible, adopting with Al is the micro Cu of active element, and trace of Al, the SnBi base solder of minipool rare earth RE can well realize the connection between sapphire.
To by micro Cu, trace of Al, the joint that the SnBi base solder ultrasonic brazing sapphire of minipool rare earth obtains carries out Mechanics Performance Testing.Fig. 6 is for when pricker material thickness is 0.5mm, and different ultrasonic amplitude welds the compression shear strength value of sapphire joint.As can be seen from the figure, when ultrasound amplitude value is 5 μm, the shear strength of joint reaches maximum, is 48Mpa.When ultrasonic amplitude is 3 μm, the average shear strength obtained is 34MPa.When amplitude is 7 μm, the average shear strength obtained is 31MPa.This is because when amplitude is less, the Al of Interface debond
2o
3nano-particle layer is thinner, and the connection of formation is more weak; And when ultrasonic amplitude is larger, solder easily splashes, thus the intensity of weld seam is declined to some extent.
Adding of mixed rare earth can significantly improve Al at Al
2o
3soaking of surface, thus Al is better combined with sapphire, simultaneously adding of mixed rare earth can the tissue of refinement Sn base solder, adopts the solder not adding mishmetal and add mishmetal to carry out ultrasonic brazing, obtains the shear strength of weld seam as shown in Figure 7.Add the weld seam shear strength after mishmetal and can bring up to 58MPa.
By fracture volume fraction be 20% nitric acid alcohol carry out eroding solder after, expose sapphire and solder interface.Observe interface by SEM and find the fine and close nano-particle layer of product, and nano particle is evenly distributed in the middle of interface, as shown in Figure 8.The size average out to 15nm of nano particle, pattern is class spheroidal.Energy spectrum analysis is carried out to it.Result shows, only containing Al, O two kinds of elements in surface resultant, and only has Al according to the most stable compound of both Al-O phasors
2o
3, therefore ultrasonic after sapphire surface generate particle be the Al that epitaxial growth goes out
2o
3, and the nano particle generated is combined well with sapphire substrates.
The cavitation of ultrasonic generation more easily occurs in interface, the instantaneous pressure produced during cavitation bubble collapse, makes the oxide-film on solder surface broken, facilitates liquid solder soaking sapphire substrates, cause interface nanometer Al
2o
3particle generates in a large number.After the oxide-film fragmentation of solder, active element Al and sapphire contact also start reaction.When just having started to contact, Al/ sapphire interface atomic arrangement schematic diagram as shown in Figure 9.Subsequently, active element Al and Al
2o
3reaction extension generates Al
2o
3the process schematic of thin layer as shown in Figure 10.
Claims (8)
1. low temperature ultrasonic SnBi base solder, it is characterized in that the chemical composition of low temperature ultrasonic SnBi base solder is by weight percentage: 41.5 ~ 52.5%Bi, 0.05 ~ 0.15%Cu, 0.01 ~ 0.1%Al, 0.01 ~ 0.05% mishmetal, surplus is Sn; Described mishmetal is that Pr forms by 50% ~ 70%Ce, 20% ~ 30%La, 10 ~ 15%Nd and surplus by weight percentage.
2. low temperature ultrasonic SnBi base solder according to claim 1, is characterized in that the chemical composition of low temperature ultrasonic SnBi base solder is by weight percentage: 49%Bi, 0.1%Cu, 0.05%Al, 0.05%RE, surplus is Sn.
3. low temperature ultrasonic SnBi base solder according to claim 1, it is characterized in that described mishmetal be by weight percentage by 55%Ce, 25%La, 12%Nd and surplus be Pr form.
4. the preparation method of low temperature ultrasonic SnBi base solder as claimed in claim 1, it is characterized in that the preparation method of low temperature ultrasonic SnBi base solder carries out in the steps below: put into by Cu in crucible, Muffle furnace is heated to 1200 DEG C, and fill Ar gas wherein, crucible is put in Muffle furnace, insulation, until Cu melts completely, in succession adds Al, Sn, Bi and mishmetal, is then incubated 20 ~ 60 minutes; Low temperature ultrasonic SnBi base solder is obtained after cooling.
5. low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or the method for ceramic matric composite as claimed in claim 1, is characterized in that the method for low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or ceramic matric composite is carried out in the steps below:
Step one, get two pieces of potteries or one piece of pottery and one block of ceramic matric composite or two blocks of ceramic matric composites as to-be-welded pieces, be placed in acetone ultrasonic cleaning;
Step 2, by low temperature ultrasonic SnBi base solder compressing tablet according to claim 1, the thickness of sheet is 0.3 ~ 0.5mm, is cut into the size corresponding with to-be-welded pieces, obtains solder sheet;
Step 3, solder sheet folder and step one in step 2 are processed rear to-be-welded pieces surface to be welded between obtain treating weldment, then will treat that weldment is put into jig and clamped;
Step 4, apply the pressure of 0.2 ~ 1Mpa, be directly pressed in by Ultrasonic probe and treat on weldment in step 3 jig, under atmospheric environment, be heated to 170 ~ 200 DEG C, applying amplitude is that the ultrasonic wave of 5 μm carries out ultrasonic wave added soldering 50 ~ 1000s.
6. low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or the method for ceramic matric composite according to claim 5, to is characterized in that in step 2 by mill milling or gets rid of band machine and rotate and get rid of band compressing tablet.
7. low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or the method for ceramic matric composite according to claim 5, is characterized in that the step one ultrasonic cleaning time is 10min.
8. low temperature ultrasonic SnBi base solder ultrasonic brazing pottery and/or the method for ceramic matric composite according to claim 5, is characterized in that the thickness of sheet in step 2 is 0.5mm.
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Cited By (5)
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| CN105237026A (en) * | 2015-11-12 | 2016-01-13 | 天津理工大学 | Ceramic/ceramic connection method for regulating and controlling middle solder layer through multi-physical-field coupling |
| CN105479030A (en) * | 2016-01-07 | 2016-04-13 | 哈尔滨工业大学 | Active anti-corrosion SnZn base brazing filler metal, manufacturing method thereof and low-temperature ultrasonic brazing method of ceramic and/or composite material and aluminum and magnesium alloy |
| CN106563861A (en) * | 2016-10-19 | 2017-04-19 | 哈尔滨工业大学（威海） | Ultrasonic soldering method for fast forming ceramic-metal interconnection |
| CN107030412A (en) * | 2017-05-17 | 2017-08-11 | 常州鑫力航金属新材料有限公司 | A kind of aluminium alloy brazing it is environmentally friendly corrosion-free from braze-welding rings and preparation method thereof |
| CN115041864A (en) * | 2022-07-08 | 2022-09-13 | 深圳市博士达焊锡制品有限公司 | High-reliability low-temperature lead-free solder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107030412A (en) * | 2017-05-17 | 2017-08-11 | 常州鑫力航金属新材料有限公司 | A kind of aluminium alloy brazing it is environmentally friendly corrosion-free from braze-welding rings and preparation method thereof |
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| CN115041864A (en) * | 2022-07-08 | 2022-09-13 | 深圳市博士达焊锡制品有限公司 | High-reliability low-temperature lead-free solder and preparation method thereof |
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