CN106736035A - The solder and method for welding of soldering 3D printing stainless steel and silicon nitride ceramics - Google Patents
The solder and method for welding of soldering 3D printing stainless steel and silicon nitride ceramics Download PDFInfo
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- CN106736035A CN106736035A CN201611252455.8A CN201611252455A CN106736035A CN 106736035 A CN106736035 A CN 106736035A CN 201611252455 A CN201611252455 A CN 201611252455A CN 106736035 A CN106736035 A CN 106736035A
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- solder
- stainless steel
- soldering
- silicon nitride
- nitride ceramics
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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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
Abstract
The invention discloses a kind of soldering 3D printing stainless steel and the solder and method for welding of silicon nitride ceramics, solder elemental composition by weight percentage includes：Cu20.0%~25.0%, In15.0%~18.0%, Ti5.0%~8.0%, Zr5.0%~10.0%, Ce0.01~0.05%, balance of Ag.The copper base solder brazing temperature that the present invention is provided is at 750 DEG C~800 DEG C, brazing filler metal melts moderate temperature, brazing filler metal melts are uniform, compared with the patent of existing this aspect, adding Zr elements can be such that the solder fusing point further reduces, Zr and Fe phase counterdiffusion simultaneously, form FeZr2, the solid solution such as Fe2Zr, Cu Zr phases are formed with Cu, with C-shaped into ZrC compounds, micro rare earth element ce can to greatest extent refine silver-based tissue, play a part of refined crystalline strengthening, above-mentioned solid solution and distributed mutually are in articulamentum and diffusion layer, ratio uniform, tissue tight, the Copper Foil in intermediate layer causes that solder has good wetability and spreadability to mother metal, the soldering joint strength of acquisition is high, corrosion resistance is good.
Description
Technical field
The present invention relates to soldering 3D printing stainless steel and the solder and method for welding of silicon nitride ceramics, belong to soldering field.
Background technology
3D printing is a kind of new RP technique, and it is built by 3 d modeling software to shape part
Mould, is cut into slices by software to threedimensional model, controls special 3D printer to enter eventually through computer export control signal
Row printing.Stainless steel has the characteristics such as corrosion-resistant, high temperature resistant and good mechanical performance.Because its powder characteristics is good, preparation technology
Simple and low cost, is very suitable for the technology of 3D printing.The stainless steel gone out with 3D printing does not cast the defect of the aspects such as fusing,
Structural constituent is uniform, good mechanical performance.Silicon nitride ceramics is a kind of excellent high temperature engineering material, and hardness is high, heat shock resistance
Property is good, and specific strength is high.The means of 3D printing stainless steel and silicon nitride ceramics soldering are coupled together, both can be played each
Advantage, the 3D printing stainless steel of matrix has preferable plasticity and toughness, can preferably resist certain impact and deformation.Silicon nitride
Ceramics can be used in the working environment of high temperature corrosion-resisting, can be used for the fields such as high temperature conjunction part.Company on stainless steel and ceramics
Method is connect, at present the main method using soldering.Chinese patent 105436741 discloses a kind of pricker for connecting metal and ceramics
Material.Its main component is silver-bearing copper indium titanium, and specific composition ratio is：Cu19.2%~28.2%, In8.2%~19.4%, Ti3.5%
~7.2%.Although the solder can successfully complete the connection of ceramics and stainless steel, because the line of ceramics and stainless steel is swollen
Swollen coefficient difference is larger, and postwelding easily produces larger stress concentration in weld layer, forms defect.
The content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention to provide a kind of soldering 3D printing stainless steel
With the solder and method for welding of silicon nitride ceramics, it is molten that on the one hand the rare earth element that the solder solder is added can play drop, refinement
The effect of crystal grain, on the other hand, the appropriate middle copper foil layer of addition can alleviate joint using the good plastic deformation of Copper Foil
Residual stress so that joint residual stress distribution is improved, and strength of joint is greatly improved.
Technical scheme：In order to solve the above technical problems, a kind of soldering 3D printing stainless steel of the invention and silicon nitride ceramics
Solder, solder elemental composition by weight percentage includes：Cu20.0%~25.0%, In15.0%~18.0%,
Ti5.0%~8.0%, Zr5.0%~10.0%, Ce0.01~0.05%, balance of Ag.
Preferably, solder elemental composition by weight percentage includes：Cu21.0%~24.0%,
In15.0%~17.0%, Ti6.0%~8.0%, Zr6.0%~9.0%, Ce0.02~0.04%, balance of Ag.
Preferably, solder elemental composition by weight percentage includes：Cu22.0%, In16.0%,
Ti7.0%, Zr8.0%, Zr8.0%, Ce0.03%, balance of Ag.
Preferably, the solder is foil-like, thickness is 60~150 μm.
A kind of method for welding of solder using above-mentioned soldering 3D printing stainless steel and silicon nitride ceramics, including following step
Suddenly：
(1) preparatory stage：3D printing stainless steel to be welded and silicon nitride ceramics sample end face are cleared up, surface is removed
Impurity, greasy dirt and oxide-film, 3D printing stainless steel is ground using W40~W7 abrasive paper for metallograph it is smooth, using W7
Number abrasive paper for metallograph by solder paillon foil and copper foil it is two-sided be ground it is smooth, by sample to be welded, solder and copper foil one after grinding
Rise and be placed in acetone, 15~20min is cleaned using ultrasonic wave, and carry out drying and processing；
(2) assembling stage：Solder and copper foil after cleaning is placed in D printing stainless steel and silicon nitride ceramics welding surface
Between, in the following order：3D printing stainless steel/solder/copper foil/solder/silicon nitride ceramics, and be close to be assemblied in special soldering
In fixture, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce the constant perpendicular of 0.05~0.08MPa
Pressure；
(3) the soldering connection stage：The fixture that will be assembled is integrally placed at the brazing equipment that vacuum is not less than 3 × 10-4Pa
In, 450~500 DEG C are warming up to the speed of 10~15 DEG C/min first, 30~40min is incubated, then with the speed of 8~10 DEG C/min
Rate is warming up to 780~820 DEG C, 20~25min of soaking time, then is cooled to 300~350 DEG C with the speed of 4~6 DEG C/min, most
After cool to room temperature with the furnace, complete welding.
Preferably, the copper foil thickness is 60~80 μm.
Beneficial effect：Compared with prior art, the present invention has advantages below：
(1) at 750 DEG C~800 DEG C, brazing filler metal melts moderate temperature, solder melts the copper base solder brazing temperature that the present invention is provided
Change uniform, compared with the patent of existing this aspect, adding Zr elements can be such that the solder fusing point further reduces, while Zr and Fe phases
Counterdiffusion, forms the solid solution such as FeZr2, Fe2Zr, and Cu-Zr phases are formed with Cu, with C-shaped into ZrC compounds, micro rare earth unit
Plain Ce can to greatest extent refine silver-based tissue, play a part of refined crystalline strengthening, and above-mentioned solid solution and distributed mutually are in articulamentum
And diffusion layer, ratio uniform, tissue tight, the Copper Foil in intermediate layer causes that solder has good wetability to mother metal and sprawls
Property, the soldering joint strength of acquisition is high, and corrosion resistance is good, can apply to completely in complex environment, is that a kind of combination property is good
Economical solder；
(2) the soldering processes advantages of simple of present invention design, using method for welding in vacuum drying oven, brazing process need not addition
Brazing flux and other safeguard measures, high vacuum environment coordinate rational processing parameter setting so that whole component without deformation, without microcosmic
Crackle, stomata and the defect such as it is mingled with, helps to obtain the soldered fitting of good mechanical properties；
(3) the rare-earth type silver-base solder that the present invention is provided has excellent normal temperature and high-temperature behavior, can fully occur with mother metal
Solid solution metallurgical reaction, can finally obtain the good connection of combination property and connect with the use of the simple and practical soldering processes of the present invention
Head.
Specific embodiment
Embodiment 1
Selection 3D printing stainless steel carries out banjo fixing butt jointing vacuum brazing with silicon nitride ceramics.Wherein 3D printing stainless steel and nitrogen
SiClx ceramic dimension is 20mm × 20mm × 5mm, and face to be brazed is 20mm × 5mm sections.
The composition and mass percent of solder are matched：Cu20.0%, In15.0%, Ti5.0%, Zr5.0%,
Ce0.01%, balance of Ag.Solder thickness is 60 μm, and copper thickness is 60 μm, and soldering process step is：
(1) preparatory stage：3D printing stainless steel to be welded and silicon nitride ceramics sample end face are cleared up, surface is removed
Impurity, greasy dirt and oxide-film, 3D printing stainless steel is ground using W40~W7 abrasive paper for metallograph it is smooth, using W7
Number abrasive paper for metallograph by solder paillon foil and copper foil it is two-sided be ground it is smooth, by sample to be welded, solder and copper foil one after grinding
Rise and be placed in acetone, 15min is cleaned using ultrasonic wave, and carry out drying and processing；
(2) assembling stage：Solder and copper foil after cleaning is placed in D printing stainless steel and silicon nitride ceramics welding surface
Between, in the following order：3D printing stainless steel/solder/copper foil/solder/silicon nitride ceramics, and be close to be assemblied in special soldering
In fixture, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce the constant perpendicular pressure of 0.05MPa；
(3) the soldering connection stage：The fixture that will be assembled is integrally placed at the brazing equipment that vacuum is not less than 3 × 10-4Pa
In, 450 DEG C are warming up to the speed of 10 DEG C/min first, 30min is incubated, then 780 DEG C are warming up to the speed of 8 DEG C/min, protect
Warm time 20min, then 300 DEG C are cooled to the speed of 4 DEG C/min, finally cool to room temperature with the furnace, complete welding.
As a result：The 3D printing stainless steel and the shaping of silicon nitride ceramics joint that soldering is obtained are good, and metallographic observation finds soldering
Area forms the interface cohesion of densification, and alloying component is evenly distributed, and room temperature shear strength is 45MPa.
Embodiment 2
3D printing stainless steel carries out banjo fixing butt jointing vacuum brazing with silicon nitride ceramics.Wherein 3D printing stainless steel and silicon nitride
Ceramic dimension is 20mm × 20mm × 5mm, and face to be brazed is 20mm × 5mm sections.
The composition and mass percent of solder are matched：Cu22.0%, In16.0%, Ti7.0%, Zr8.0%,
Ce0.03%, balance of Ag.The solder thickness of offer is 80 μm, and copper thickness is 70 μm, and soldering process step is：
(1) preparatory stage：3D printing stainless steel to be welded and silicon nitride ceramics sample end face are cleared up, surface is removed
Impurity, greasy dirt and oxide-film, 3D printing stainless steel is ground using W40~W7 abrasive paper for metallograph it is smooth, using W7
Number abrasive paper for metallograph by solder paillon foil and copper foil it is two-sided be ground it is smooth, by sample to be welded, solder and copper foil one after grinding
Rise and be placed in acetone, 18min is cleaned using ultrasonic wave, and carry out drying and processing；
(2) assembling stage：Solder and copper foil after cleaning is placed in D printing stainless steel and silicon nitride ceramics welding surface
Between, in the following order：3D printing stainless steel/solder/copper foil/solder/silicon nitride ceramics, and be close to be assemblied in special soldering
In fixture, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce the constant perpendicular pressure of 0.06MPa；
(3) the soldering connection stage：The fixture that will be assembled is integrally placed at the brazing equipment that vacuum is not less than 3 × 10-4Pa
In, 480 DEG C are warming up to the speed of 12 DEG C/min first, 35min is incubated, then 800 DEG C are warming up to the speed of 9 DEG C/min, protect
Warm time 22min, then 320 DEG C are cooled to the speed of 5 DEG C/min, finally cool to room temperature with the furnace, complete welding.
As a result：The 3D printing stainless steel and the shaping of silicon nitride ceramics joint that soldering is obtained are good, and metallographic observation finds soldering
Area forms the interface cohesion of densification, and alloying component is evenly distributed, and room temperature shear strength is 47MPa.
Embodiment 3
Selection 3D printing stainless steel carries out banjo fixing butt jointing vacuum brazing with silicon nitride ceramics.Wherein 3D printing stainless steel and nitrogen
SiClx ceramic dimension is 20mm × 20mm × 5mm, and face to be brazed is 20mm × 5mm sections.
The composition and mass percent of solder are matched：Cu25.0%, In18.0%, Ti8.0%, Zr10.0%,
Ce0.05%, balance of Ag.The solder thickness of offer is 150 μm, and copper thickness is 80 μm.
Soldering process step is：
(1) preparatory stage：3D printing stainless steel to be welded and silicon nitride ceramics sample end face are cleared up, surface is removed
Impurity, greasy dirt and oxide-film, 3D printing stainless steel is ground using W40~W7 abrasive paper for metallograph it is smooth, using W7
Number abrasive paper for metallograph by solder paillon foil and copper foil it is two-sided be ground it is smooth, by sample to be welded, solder and copper foil one after grinding
Rise and be placed in acetone, 20min is cleaned using ultrasonic wave, and carry out drying and processing；
(2) assembling stage：Solder and copper foil after cleaning is placed in D printing stainless steel and silicon nitride ceramics welding surface
Between, in the following order：3D printing stainless steel/solder/copper foil/solder/silicon nitride ceramics, and be close to be assemblied in special soldering
In fixture, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce the constant perpendicular pressure of 0.08MPa；
(3) the soldering connection stage：The fixture that will be assembled is integrally placed at the brazing equipment that vacuum is not less than 3 × 10-4Pa
In, 500 DEG C are warming up to the speed of 15 DEG C/min first, 40min is incubated, then 820 DEG C are warming up to the speed of 10 DEG C/min, protect
Warm time 25min, then 350 DEG C are cooled to the speed of 6 DEG C/min, finally cool to room temperature with the furnace, complete welding.
As a result：The 3D printing stainless steel and the shaping of silicon nitride ceramics joint that soldering is obtained are good, and metallographic observation finds soldering
Area forms the interface cohesion of densification, and alloying component is evenly distributed, and room temperature shear strength is 49MPa.
Embodiment 4
Selection 3D printing stainless steel carries out banjo fixing butt jointing vacuum brazing with silicon nitride ceramics.Wherein 3D printing stainless steel and nitrogen
SiClx ceramic dimension is 20mm × 20mm × 5mm, and face to be brazed is 20mm × 5mm sections.
The composition and mass percent of solder are matched：Cu21.0%, In15.0%, Ti6.0%, Zr6.0%,
Ce0.02%, balance of Ag.The solder thickness of offer is 150 μm, and copper thickness is 80 μm.
Soldering processes are same as Example 1.
As a result：The 3D printing stainless steel and the shaping of silicon nitride ceramics joint that soldering is obtained are good, and metallographic observation finds soldering
Area forms the interface cohesion of densification, and alloying component is evenly distributed, and room temperature shear strength is 46MPa.
Embodiment 5
Selection 3D printing stainless steel carries out banjo fixing butt jointing vacuum brazing with silicon nitride ceramics.Wherein 3D printing stainless steel and nitrogen
SiClx ceramic dimension is 20mm × 20mm × 5mm, and face to be brazed is 20mm × 5mm sections.
The composition and mass percent of solder are matched：Cu24.0%, In17.0%, Ti8.0%, Zr9.0%,
Ce0.04%, balance of Ag.The solder thickness of offer is 150 μm, and copper thickness is 80 μm.
Soldering processes are same as Example 1.
As a result：The 3D printing stainless steel and the shaping of silicon nitride ceramics joint that soldering is obtained are good, and metallographic observation finds soldering
Area forms the interface cohesion of densification, and alloying component is evenly distributed, and room temperature shear strength is 47MPa.
Comparative example
Compared with Example 1, only the composition of solder is different, and solder is as shown in table 1：
Table 1
As shown in Table 1, soldered fitting dense micro-structure obtained in embodiment 1-3, is uniformly distributed, and linkage interface is obvious,
Shear strength is between 45-49MPa, it can thus be appreciated that solder tool of the present invention for soldering 3D printing stainless steel and silicon nitride ceramics
Standby good adhesive force and wettability, and soldered fitting bond strength is high.
Comparative example 1 shows：Appropriate copper effectively can form solid solution knot with the element in mother metal, solder
Close, be conducive to the formation of joint, lacking copper can cause joint cracking or even cannot burn-on.Comparative example 2 shows：Solder
In rare earth element indium can effectively improve wetability of the solder to mother metal, crystal grain thinning improves strength of joint.Contrast is implemented
Example 3 shows：Appropriate Ti can improve wetting of the solder to mother metal, while forming solid solution with other elements in mother metal and solder
Body, it is ensured that joint reaches metallurgical binding.Comparative example 4 shows：Micro Zr can form the solid solution such as FeZr2, Fe2Zr,
Cu-Zr phases are formed with Cu, with C-shaped into ZrC compounds, improves the mechanical property of joint so that dense structure.Certain above-mentioned element
There is appropriate scope to limit, when Ti, Zr too high levels, be also easy to produce substantial amounts of frangible compounds, reduce the mechanical property of joint
Energy.Copper content is too high to be caused to extrude the solder of part fusing in brazing process, influence the formation of joint.
The above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (6)
1. the solder of a kind of soldering 3D printing stainless steel and silicon nitride ceramics, it is characterised in that：Solder is by weight percentage
Elemental composition includes：Cu20.0%~25.0%, In15.0%~18.0%, Ti5.0%~8.0%, Zr5.0%~
10.0%, Ce0.01~0.05%, balance of Ag.
2. the solder of soldering 3D printing stainless steel according to claim 1 and silicon nitride ceramics, it is characterised in that：The pricker
Material elemental composition by weight percentage includes：Cu21.0%~24.0%, In15.0%~17.0%, Ti6.0%~
8.0%, Zr6.0%~9.0%, Ce0.02~0.04%, balance of Ag.
3. the solder of soldering 3D printing stainless steel according to claim 1 and silicon nitride ceramics, it is characterised in that：The pricker
Material elemental composition by weight percentage includes：Cu22.0%, In16.0%, Ti7.0%, Zr8.0%, Zr8.0%,
Ce0.03%, balance of Ag.
4. the solder of soldering 3D printing stainless steel according to claim 1 and silicon nitride ceramics, it is characterised in that：The pricker
Expect to be foil-like, thickness is 60~150 μm.
5. soldering 3D printing stainless steel and the pricker of the solder of silicon nitride ceramics described in a kind of any one of utilization claim 1 to 4
Soldering method, it is characterised in that comprise the following steps：
(1) preparatory stage：3D printing stainless steel to be welded and silicon nitride ceramics sample end face are cleared up, the miscellaneous of surface is removed
Matter, greasy dirt and oxide-film, 3D printing stainless steel is ground using W40~W7 abrasive paper for metallograph it is smooth, using W7 gold
Phase sand paper is ground smooth by solder paillon foil and copper foil are two-sided, puts sample to be welded, solder and copper foil together after grinding
In acetone, 15~20min is cleaned using ultrasonic wave, and carry out drying and processing；
(2) assembling stage：By the solder and copper foil after cleaning be placed in D printing stainless steel and silicon nitride ceramics welding surface it
Between, in the following order：3D printing stainless steel/solder/copper foil/solder/silicon nitride ceramics, and be close to be assemblied in special soldering folder
In tool, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce the constant perpendicular pressure of 0.05~0.08MPa
Power；
(3) the soldering connection stage：The fixture that will be assembled is integrally placed at vacuum and is not less than in the brazing equipment of 3 × 10-4Pa,
450~500 DEG C are warming up to the speed of 10~15 DEG C/min first, 30~40min is incubated, then with the speed of 8~10 DEG C/min
It is warming up to 780~820 DEG C, 20~25min of soaking time, then 300~350 DEG C are cooled to the speed of 4~6 DEG C/min, finally
Cool to room temperature with the furnace, complete welding.
6. the method for welding of the solder of utilization soldering 3D printing stainless steel according to claim 5 and silicon nitride ceramics, its
It is characterised by：The copper foil thickness is 60~80 μm.
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| CN108480876A (en) * | 2018-03-30 | 2018-09-04 | 西安瑞鑫科金属材料有限责任公司 | A kind of silver-base solder for zirconia ceramics and solder bonding metal |
| CN111761155A (en) * | 2020-06-01 | 2020-10-13 | 中国电子科技集团公司第十四研究所 | Novel preparation method of integrated water hinge friction pair |
| CN114309853A (en) * | 2021-12-22 | 2022-04-12 | 无锡天杨电子有限公司 | Buffer welding method for thick SiC ceramic part and thick stainless steel part |
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| CN105618957A (en) * | 2016-03-10 | 2016-06-01 | 江苏科技大学 | Solder used for vacuum active brazing process of W-Cu composite material and stainless steel and method |
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| CN108480876A (en) * | 2018-03-30 | 2018-09-04 | 西安瑞鑫科金属材料有限责任公司 | A kind of silver-base solder for zirconia ceramics and solder bonding metal |
| CN111761155A (en) * | 2020-06-01 | 2020-10-13 | 中国电子科技集团公司第十四研究所 | Novel preparation method of integrated water hinge friction pair |
| CN114309853A (en) * | 2021-12-22 | 2022-04-12 | 无锡天杨电子有限公司 | Buffer welding method for thick SiC ceramic part and thick stainless steel part |
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