CN104889594B - Low temperature ultrasonic SnBi base solders and preparation method thereof, and its ultrasonic brazing ceramics and/or ceramic matric composite method - Google Patents
Low temperature ultrasonic SnBi base solders and preparation method thereof, and its ultrasonic brazing ceramics and/or ceramic matric composite method Download PDFInfo
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- CN104889594B CN104889594B CN201510306294.5A CN201510306294A CN104889594B CN 104889594 B CN104889594 B CN 104889594B CN 201510306294 A CN201510306294 A CN 201510306294A CN 104889594 B CN104889594 B CN 104889594B
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Classifications
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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
-
- 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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- Chemical & Material Sciences (AREA)
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- Ceramic Products (AREA)
Abstract
Low temperature ultrasonic SnBi base solders and preparation method thereof, and its ultrasonic brazing ceramics and/or ceramic matric composite method；It belongs to the soldering tech field of ceramics and ceramic matric composite.The present invention solves prior art can only soldering at high temperature, it is difficult to form the problem of residual thermal stress formed in effectively connection, cooling procedure causes weld cracking.Low temperature ultrasonic SnBi base solders Bi, Cu, Al, mischmetal (RE) and Sn compositions, preparation method：Ar gas is filled Muffle stove heat and thereto, the crucible for filling Cu is put into wherein, insulation is melted completely to Cu, be sequentially added Al, Sn, Bi and mischmetal, be incubated 20~60min.Method for welding：Apply pressure, Ultrasonic probe is directly pressed on the part to be welded in fixture, under atmospheric environment, be heated to 170~200 DEG C, apply ultrasonic brazing.The present invention is used for ultrasonic brazing and connects ceramics and/or ceramic matric composite.
Description
Technical field
The invention belongs to the soldering tech field of structural ceramics and its composite, and in particular to a kind of low temperature ultrasonic SnBi
Base solder and preparation method thereof, and ultrasonic brazing ceramics and/or ceramic matric composite method.
Background technology
The high mechanical strength, good with preferable wearability, corrosion resistance, and thermal stability of ceramics.Sapphire is
The most frequently used one kind in ceramics.
Sapphire is widely used in optics and window material due to its preferable optical property.However as existing
For demand of the optical system to high-aperture optical material, the sapphire size obtained by Artificial Growth can not meet need
Ask.At present, the unique channel for acquiring large scale optical window is exactly by the way that fritter sapphire is connected together.Therefore, it is blue
The interconnection technique of jewel has become the focus of academia's words, with important research and practical value.
Sapphire is connected because the macromolecule in joint is easily decomposed at high temperature and is existed certain reliable by bonded process
Sex chromosome mosaicism, and bonding strength is not high.There is the defects such as hole in the weld seam that reaction sintering is obtained, as sapphire fracture process
In crack source.Soldering is to realize that ceramic material connects most common method, the sapphire activity of soldering being widely used at present
Solder is mainly Ag-Cu-Ti solders.By active element Ti and sapphire reaction, promote liquid solder and sapphire profit
Wet combination.Whole welding process needs that in vacuum environment and 850 DEG C of high temperature connection could be realized, is cooled to from high temperature (850 DEG C)
During room temperature, because solder with sapphire thermal coefficient of expansion differs larger, welding point is caused to leave very big remnants
Stress, the main cause as Joint Cracking.
The content of the invention
The invention solves the problems that can only be in high temperature (850 using existing active solder ceramic soldering and/or ceramic matric composite
DEG C) under soldering, and be difficult to be formed the problem of weld cracking is caused due to residual thermal stress in effectively connection, cooling procedure；
And it is ceramic and/or ceramic matric composite there is provided low temperature ultrasonic SnBi base solders and preparation method thereof, and its ultrasonic brazing
Method.
In order to solve the above technical problems, the chemical composition of low temperature ultrasonic SnBi base solders is by weight percentage in the present invention
For：The mischmetal of 41.5~52.5%Bi, 0.05~0.15%Cu, 0.01~0.1%Al, 0.01~0.05%, surplus is Sn；
The mischmetal be by weight percentage by 50%~70%Ce, 20%~30%La, 10~15%Nd and surplus be Pr groups
Into；Its preparation method is carried out in the steps below：Cu is put into crucible, Muffle furnace is heated to 1200 DEG C, and to its
In fill Ar gas, crucible is put into Muffle furnace, insulation is melted until Cu completely, is sequentially added Al, Sn, Bi and mischmetal
RE, is then incubated 20~60 minutes；Low temperature ultrasonic SnBi base solders are obtained after cooling.
The method of low temperature ultrasonic SnBi base solders ultrasonic brazing ceramics and/or ceramic matric composite is to enter in the steps below
Capable：
Step 1: taking two pieces of ceramics or one piece of ceramics and one block of ceramic matric composite or two pieces of ceramic base composite woods
Material is placed in acetone and is cleaned by ultrasonic as to-be-welded pieces；
Step 2: by low temperature ultrasonic SnBi base solder compressing tablets, the thickness of piece is 0.3~0.5mm, is cut into and to-be-welded pieces
Corresponding size, obtains solder piece；
Step 3: obtaining to be welded between the surface to be welded of to-be-welded pieces after solder piece folder and step one in step 2 are handled
Part, is then put into clamping in fixture by part to be welded；
Step 4: applying 0.2~1Mpa pressure, Ultrasonic probe is directly born against into the part to be welded in step 3 fixture
On, under atmospheric environment, be heated to 170~200 DEG C, apply amplitude for 5 μm of ultrasonic wave carry out ultrasonic wave added soldering 50~
1000s。
The present invention use using Al elements as active element SnBi base solders, realize at a lower temperature (170~
200 DEG C) ultrasonic brazing connection ceramic (sapphire) and containing ceramic matric composite etc., the composite containing ceramic base is as contained pottery
Glass, silicon, aluminium alloy, magnesium alloy, titanium alloy of porcelain particle etc..Present invention, avoiding the cracking of joint, realize ceramics and/or
Effective connection of ceramic matric composite, particularly sapphire welding.
Compared with prior art the advantage of the invention is that：
1st, the present invention is using Al as ceramic soldering and/or the active element of ceramic matric composite, by Al to ceramic and/or
Ceramic matric composite diffusion into the surface reaction generation Al2O3Excessive layer, realizes ceramics and/or ceramic matric composite substrate and pricker
Effective connection of material.
2nd, Al content is micro content (0.01%-0.1%) in the present invention, and Al fusing point is 660 DEG C, and trace of Al can be kept away
The fusing point for exempting from Sn base solders significantly rises, while avoiding Al and the Cu reaction generations CuAl in solder2, CuAl and Cu2The fragility such as Al
Intermetallic compound, so as to weaken weld seam.
3rd, Cu elements can be with the Sn elements formation Cu in solder in the present invention6Sn5, the Cu of generation6Sn5As nucleating agent, increase
The big nucleation rate of SnBi eutectic structures, promotes the refinement of β-Sn phases and richness Bi phase crystal grain, improves the fragility of solder.Solder
Elongation brought up to 39% from be not added with Cu elements 21%.
4th, the Cu elements added in the present invention are in weld seam forming process, the Cu of generation6Sn5, so that crystal grain thinning.Weld seam
The refinement of crystal grain can improve toughness in tissue, residual stress be reduced, so that the intensity of weld seam has been lifted.
5th, present invention SnBi containing low temperature ultrasonic base solders realize low-temperature welding, reduce in cooling procedure because structure is made pottery
The residual stress that the thermal coefficient of expansion of porcelain and solder is mismatched and produced, so that greatly reinforcing structural ceramics weldment is using process
In reliability.And during existing active solder (Ag-Cu-Ti solders) is using Ti as the welding of active element, due to brazing temperature compared with
Height, causes welding point residual stress in cooling procedure larger, in use in the presence of certain reliability the problem of.
6th, low temperature ultrasonic SnBi base solders ultrasonic brazing of the invention ceramics and/or ceramic matric composite are in atmospheric environment
In can be achieved with effectively connection.And existing active solder (Ag-Cu-Ti solders) ceramic soldering and/or ceramic matric composite are needed
To carry out in a vacuum furnace, the requirement to welding surroundings is harsher.
7th, Ti's is expensive, and Al less expensive, and the present invention uses Al as active element reduction production pricker
The cost of material.
8th, the addition of mixed rare earth can significantly improve Al in Al2O3The wetting on surface, so that Al and ceramics or ceramics
Can preferably it be combined between particle, while the addition of mixed rare earth can refine the tissue of Sn base solders.
Brief description of the drawings
Fig. 1 is ultrasonic wave added soldering sapphire schematic diagram；Fig. 2 is the DSC curve of low temperature ultrasonic SnBi base solders；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 bases solder is closed；Fig. 5 is welding point group
Knit pattern；Fig. 6 is change of the welding point shear strength with ultrasonic amplitude；Fig. 7 is that mischmetal adds Welded Joints shearing
The influence of intensity；Fig. 8 is the nanometer Al of sapphire/solder interface generation2O3Particle SEM image；Fig. 9 be active element Al with
Al2O3Interracial contact atomic arrangement schematic diagram；Figure 10 is active element Al and Al2O3React epitaxial growth Al2O3Thin layer schematic diagram；
1 in wherein Fig. 1 --- upper sapphire to be welded, 2 --- lower sapphire to be welded, 3 --- solder, 4 --- Ultrasonic probe,
5 --- heating coil, 6 --- fixing mould, 7 --- variable-sized fixtures.
Embodiment
Embodiment one：The chemical composition of low temperature ultrasonic SnBi base solders is shown in Table 1 in present embodiment：
Table 1 is the chemical composition (by weight percentage) of low temperature ultrasonic SnBi base solders
Wherein, the chemical composition of minipool rare earth (RE) is shown in Table 2：
Table 2 is the chemical composition (by weight percentage) of mischmetal (RE)
The preparation method of low temperature ultrasonic SnBi base solders is as follows in present embodiment：
Cu is put into crucible, Muffle furnace is heated to 1200 DEG C, and fills Ar gas thereto, crucible is put into Muffle
In stove, insulation is melted completely until Cu, is sequentially added Al, Sn, Bi and mixed rare earth, is then incubated 30 minutes；After cooling
Obtain low temperature ultrasonic SnBi base solders.
Low temperature ultrasonic SnBi bases solder ultrasonic brazing sapphire method is carried out in the steps below in present embodiment：
It is cleaned by ultrasonic 10min Step 1: sapphire to be welded is placed in acetone；
Step 2: low temperature ultrasonic SnBi base solders are by mill milling, or carry out compressing tablet by getting rid of to get rid of in band with machine rotation,
Pricker material thickness is measured with spiral micrometer, until pricker material thickness is 0.5mm, and 10cm × 10cm size is cut into；
Step 3: constituting and treating between two pieces of sapphire surfaces to be welded after solder piece folder and step one in step 2 are handled
Weldment, is then put into clamping in fixture by part to be welded；
Step 4: applying 0.2Mpa pressure, Ultrasonic probe is directly born against on the sapphire weldment in step 3 fixture,
Under atmospheric environment, 170 DEG C are heated to, ultrasonic amplitude is set as 5 μm, ultrasonic wave application time is 50s, carries out ultrasonic wave added pricker
Weldering, as shown in Figure 1.
The low temperature ultrasonic SnBi base solder liquidus temperatures of present embodiment are accurately measured, heating differential analysis are carried out,
As a result it is as shown in Figure 2.Learnt by curve, 143.8 DEG C of solder solidus, 155.8 DEG C of liquidus curve.Generally, brazing temperature is liquid
More than liquidus temperature ten several years.So brazing temperature is set as 170 DEG C, solder can soldering sapphire at low temperature.
The microstructure SEM figures of low temperature ultrasonic SnBi base solder liquid alloys are as shown in Figure 3.Wherein, grey form and aspect are richness Bi phases
And the rich Bi phases of secondary precipitation, it is light for β-Sn phases.Richness Bi phases crystal grain is observed that from SEM figures and its thick, led
Cause the brazing filler metal alloy fragility very big.And when the addition of micro Cu in solder, the rich Bi phases in solder are refined, such as scheme
Shown in 4 SEM figures.This is due to Cu meetings and the Sn reaction generations Cu of addition6Sn5.What weld seam was separated out first in process of setting is
High temperature Cu6Sn5Phase (415 DEG C of fusing point), Cu6Sn5Play a part of nucleating agent, increase the nucleation rate of SnBi eutectic structures, so that
Promote the refinement of β-Sn phases and richness Bi phases.And the refinement of β-Sn phases and richness Bi phases adds the ductility of solder.
The tissue topography of joint is as shown in Figure 5 after ultrasonic brazing.Ultrasonic brazing is carried out using low temperature ultrasonic SnBi bases solder,
Postwelding, solder is tightly combined with sapphire substrates, without obvious weld defect.It can be seen that, use using Al as the micro- of active element
Cu is measured, trace of Al, minipool rare earth RE SnBi base solders can be very good to realize the connection between sapphire.
To with micro Cu, trace of Al, the joint that the SnBi base solder ultrasonic brazing sapphires of minipool rare earth are obtained enters
Row Mechanics Performance Testing.Fig. 6 is that, when pricker material thickness is 0.5mm, the compression shear of different ultrasonic amplitude welding sapphire joints is strong
Angle value.It can be seen that when ultrasound amplitude value is 5 μm, the shear strength of joint reaches maximum, is 48Mpa.When super
When sound and vibration width is 3 μm, obtained average shear strength is 34MPa.When amplitude is 7 μm, obtained average shear strength is
31MPa.Because when amplitude is smaller, the Al of interface generation2O3Nano-particle layer is relatively thin, and the connection of formation is weaker；And when super
When sound and vibration is larger, solder easily splashes, so that the intensity of weld seam has declined.
The addition of mixed rare earth can significantly improve Al in Al2O3The wetting on surface, so that Al can be more with sapphire
Good combination, while the addition of mixed rare earth can refine the tissue of Sn base solders, using being added without mischmetal and addition
The solder of mischmetal carries out ultrasonic brazing, and the shear strength for obtaining weld seam is as shown in Figure 7.Plus the weld seam shearing after mischmetal
Intensity can bring up to 58MPa.
Fracture for 20% nitric acid alcohol erode after solder with volume fraction, exposes sapphire and solder circle
Face.The fine and close nano-particle layer of product is found by SEM observing interfaces, and nano particle is evenly distributed in interface and worked as
In, 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.As a result table
It is bright, two kinds of elements of Al, O are comprised only in surface resultant, and Al is only had according to the most stable of compound of both Al-O phasors2O3, therefore
The Al that the particle generated after ultrasound in sapphire surface goes out for epitaxial growth2O3, and the nano particle and sapphire substrates generated
It is well combined.
The cavitation that ultrasound is produced more readily occurs in interface, and the instantaneous pressure that cavitation bubble is produced when collapsing makes solder table
The oxide-film in face is crushed, and promotes wetting of the liquid solder to sapphire substrates, causes interface nanometer Al2O3Particle is largely given birth to
Into.After the oxide-film of solder is broken, active element Al and sapphire contact simultaneously start reaction.When just starting contact, Al/ is blue precious
Stone interface atoms arrangement schematic diagram is as shown in Figure 9.Then, active element Al and Al2O3React extension generation Al2O3The mistake of thin layer
Journey schematic diagram is as shown in Figure 10.
Claims (3)
1. the preparation method of low temperature ultrasonic SnBi base solders, it is characterised in that the preparation method of low temperature ultrasonic SnBi base solders be by
What following step was carried out：Cu is put into crucible, Muffle furnace is heated to 1200 DEG C, and fills Ar gas thereto, crucible is put
Enter into Muffle furnace, insulation is melted completely until Cu, is sequentially added Al, Sn, Bi and mischmetal, be then incubated 20~60 points
Clock；Low temperature ultrasonic SnBi base solders are obtained after cooling, the chemical composition of the low temperature ultrasonic SnBi base solders is with percentage by weight
It is calculated as：The mischmetal of 41.5~52.5%Bi, 0.05~0.15%Cu, 0.01~0.1%Al, 0.01~0.05%, surplus is
Sn；The mischmetal be by weight percentage by 50%~70%Ce, 20%~30%La, 10~15%Nd and surplus be Pr
Composition.
2. the preparation method of low temperature ultrasonic SnBi base solders according to claim 1, it is characterised in that the low temperature ultrasonic
The chemical composition of SnBi base solders is by weight percentage：49%Bi, 0.1%Cu, 0.05%Al, 0.05% mischmetal,
Surplus is Sn.
3. the preparation method of low temperature ultrasonic SnBi base solders according to claim 1, it is characterised in that the mischmetal
It is that, by 55%Ce, 25%La, 12%Nd and surplus constitute for Pr by weight percentage.
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| CN105237026B (en) * | 2015-11-12 | 2017-06-20 | 天津理工大学 | A kind of ceramics/ceramic joining method of multiple physical field coupling regulation and control intermediate solder layer |
| 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 |
| CN107030412B (en) * | 2017-05-17 | 2019-12-10 | 常州鑫力航金属新材料有限公司 | environment-friendly corrosion-free self-brazing ring for aluminum alloy brazing 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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| US5368814A (en) * | 1993-06-16 | 1994-11-29 | International Business Machines, Inc. | Lead free, tin-bismuth solder alloys |
| US6156132A (en) * | 1998-02-05 | 2000-12-05 | Fuji Electric Co., Ltd. | Solder alloys |
| JP4338854B2 (en) * | 1999-11-25 | 2009-10-07 | 三井金属鉱業株式会社 | Tin-bismuth lead-free solder |
| CN101081464A (en) * | 2007-07-13 | 2007-12-05 | 北京工业大学 | SnBi and SnBiAg series low-temperature leadless solder containing trace quantity of rare-earth |
| CN102260088A (en) * | 2011-06-28 | 2011-11-30 | 哈尔滨工业大学 | Low-stress low-temperature ceramic brazing method |
| EP3907037A1 (en) * | 2011-08-02 | 2021-11-10 | Alpha Assembly Solutions Inc. | High impact toughness solder alloy |
| KR102087004B1 (en) * | 2012-03-20 | 2020-03-10 | 알파 어셈블리 솔루션스 인크. | Solder preforms and solder alloy assembly methods |
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