CN114043026B - Stress relieving method in ceramic-metal - Google Patents
Stress relieving method in ceramic-metal Download PDFInfo
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- CN114043026B CN114043026B CN202111340811.2A CN202111340811A CN114043026B CN 114043026 B CN114043026 B CN 114043026B CN 202111340811 A CN202111340811 A CN 202111340811A CN 114043026 B CN114043026 B CN 114043026B
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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
- 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
-
- 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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application provides a stress relieving method in ceramic-metal, which relates to the technical field of material welding and comprises the following steps: coating soft solder on the surface to be welded of the porous ceramic base material, so that the soft solder is filled into the gaps of the surface to be welded of the porous ceramic base material, and obtaining a modified porous ceramic base material filled with the soft solder; and (3) coating hard brazing filler metal on the surface of the treated metal base metal, sequentially placing the metal base metal, the hard brazing filler metal and the modified porous ceramic base metal according to the sequence, clamping by using a die, and sending the die into a vacuum furnace for heat treatment to finish ceramic-metal connection. The application realizes the effective control of the distribution of soft solder and hard solder by a two-step method so as to simultaneously ensure the temperature resistance and the stress release of the ceramic-metal joint.
Description
Technical Field
The application relates to the technical field of material welding, in particular to a stress relieving method in ceramic-metal.
Background
The connection of ceramics to metals provides feasibility for the preparation of new structural members of large size and complex shape and therefore, is a hot spot of concern to researchers. At present, one of the problems of welding ceramics and metals is that the difference of the thermal expansion coefficients of the ceramics and the metals is large, namely, large joint thermal stress exists.
In the prior art, a common method for relieving residual stress comprises the following steps: soft base solder; soft particle reinforced phase/interlayer; a gradient intermediate layer; low temperature welding and high temperature use, etc. For example, some use of an AuCu/Mo/AuCu interlayer for relieving stress of GH536 and SiCf/SiC, plastic deformation of the AuCu layer effectively improves the interlayer's ability to relieve residual stress; the AgCuTi is directly used as a brazing filler metal to realize the welding of ceramics and metals, but the AgCuTi has the problem of high-temperature softening, so that the temperature resistance of the joint is greatly reduced. While common hard solders, such as TiNix, tiZrNiCu, al—ti solders, have little problem of softening at high temperatures, their ability to release stresses is weak relative to soft solders.
Disclosure of Invention
The application solves the problem that the method for relieving the residual stress in the prior art cannot ensure the temperature resistance of the joint.
In order to solve the above problems, the present application provides a stress relief method in ceramic-metal, comprising:
step S1, coating soft solder on a surface to be welded of a porous ceramic base material, and filling the soft solder into a gap of the surface to be welded of the porous ceramic base material to obtain a modified porous ceramic base material filled with the soft solder;
and S2, coating hard brazing filler metal on the surface of the treated metal base metal, sequentially placing the metal base metal, the hard brazing filler metal and the modified porous ceramic base metal in sequence, clamping by using a die, and sending the die into a vacuum furnace for heat treatment to finish ceramic-metal connection.
Preferably, in step S2, the heat treatment process includes: heating to 350-450 ℃ at 9-11 ℃/min, preserving heat for 8-10min, continuing heating to the brazing temperature of the hard brazing filler metal at 9-11 ℃/min, preserving heat for 5-15min, melting the hard brazing filler metal, cooling to 350-450 ℃ at 7-8 ℃/min, closing heating, and cooling to room temperature in a furnace.
Preferably, the brazing temperature of the brazing filler metal is 50-200 ℃ lower than the melting point of the soft brazing filler metal.
Preferably, the hard solder comprises BNi7 (Ni-Cr- (P)) paste, tiNi paste or TiZrNiCu amorphous foil tape.
Preferably, the BNi7 (Ni-Cr- (P)) paste is obtained by mixing commercial BNi7 (Ni-Cr- (P)) powder with a first binder, and the TiNi paste is obtained by mixing TiNi powder with a second binder.
Preferably, in step S1, the coating the soft solder on the surface to be welded of the porous ceramic base material includes:
s11, preparing soft solder paste;
and step S12, coating the soft solder paste on the surface to be welded of the processed porous ceramic base material in a screen printing mode, performing heat treatment in a vacuum furnace, and obtaining the modified porous ceramic base material after post-treatment.
Preferably, the solder paste in step S11 is obtained by mixing solder powder with a third binder.
Preferably, the solder powder is selected from the group consisting of Ag-Ti powder, ag-V powder, au-Ti powder and Cu-Si powder.
Preferably, the third adhesive comprises a mixture of terpineol and absolute ethyl alcohol, and the volume ratio of the terpineol to the absolute ethyl alcohol is 5 (1-5).
Preferably, in step S12, the heat treatment process includes: heating to 350-450 ℃ at 9-11 ℃/min, preserving heat for 8-10min, continuing heating to melt the soft solder at 9-11 ℃/min, cooling to 350-450 ℃ at 7-8 ℃/min, and turning off the heating and cooling to room temperature.
The stress relief method in the ceramic-metal of the application has the advantages compared with the prior art that: the application realizes the effective control of the distribution of soft solder and hard solder by a two-step method so as to simultaneously ensure the temperature resistance and the stress release of the ceramic-metal joint. Specifically, the soft solder is prefabricated in the gaps of the to-be-welded surface of the porous ceramic base material, and is controlled in the gaps of the ceramic surface instead of the welding layer, so that on one hand, the problem of softening caused by soft metal in high-temperature use can be avoided, and on the other hand, the soft solder in direct contact with the porous ceramic can effectively relieve the residual stress of the joint through plastic deformation. Secondly, the modified porous ceramic base metal and the metal base metal are connected through the hard brazing filler metal with relatively better temperature resistance, so that the modified porous ceramic base metal and the metal base metal are effectively connected, and certain temperature resistance can be ensured.
Drawings
FIG. 1 is a flow chart of a method of stress relief in a ceramic-metal in an embodiment of the application;
FIG. 2 is an assembly schematic of the stress relief method in ceramic-metal of example 1 of the present application;
FIG. 3 is a schematic diagram showing the stress distribution of the ceramic-metal joint obtained in example 1 of the present application;
FIG. 4 is a schematic diagram showing the stress distribution of the ceramic-metal joint obtained in example 2 of the present application.
Detailed Description
In order that the above objects, features and advantages of the application will be readily understood, a more particular description of the application will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
The terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", and "a third" may explicitly or implicitly include at least one such feature.
In the description of embodiments of the present application, the term "description of some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms do not necessarily refer to the same implementations or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
As shown in fig. 1, an embodiment of the present application provides a method for relieving stress in ceramic-metal, including:
step S1, coating soft solder on a surface to be welded of a porous ceramic base material, and filling the soft solder into a gap of the surface to be welded of the porous ceramic base material to obtain a modified porous ceramic base material filled with the soft solder;
and S2, coating hard brazing filler metal on the surface of the treated metal base metal, sequentially placing the metal base metal, the hard brazing filler metal and the modified porous ceramic base metal in sequence, clamping by using a die, and sending the die into a vacuum furnace for heat treatment to finish ceramic-metal connection.
In some preferred embodiments, in step S2, the heat treatment process includes: heating to 350-450 ℃ at 9-11 ℃/min for 8-10min, which is favorable for volatilization of the adhesive terpineol, continuously heating to the brazing temperature of the hard brazing filler metal at 9-11 ℃/min, and keeping the temperature for 5-15min to melt the hard brazing filler metal, then cooling to 350-450 ℃ at 7-8 ℃/min, closing heating, and cooling to room temperature.
In some embodiments, the braze needs to be able to react with the ceramic/metal base material or be well-wetting with the ceramic/metal to achieve an effective ceramic/metal connection.
In some embodiments, the braze has a braze temperature that is 50-200 ℃ below the melting point of the braze. Therefore, the hard solder cannot excessively damage the soft solder prefabricated in the holes due to the excessively high temperature in the melting and brazing process, so that the soft solder is melted in a large amount and is diffused into the whole welding seam. When the brazing temperature of the hard brazing filler metal is slightly lower than the melting point of the soft brazing filler metal (50-200 ℃), on one hand, the soft brazing filler metal can be ensured not to be dissolved and diffused in a large amount in the heat treatment process of the step S2; on the other hand, it is also possible to ensure a certain temperature resistance of the final joint, since the hard solder hardly softens before reaching the melting point.
In some embodiments, in step S1, the coating the soft solder on the surface to be soldered of the porous ceramic base material includes:
s11, preparing soft solder paste;
and step S12, coating the soft solder paste on the surface to be welded of the processed porous ceramic base material in a screen printing mode, performing heat treatment in a vacuum furnace, and obtaining the modified porous ceramic base material after post-treatment.
Therefore, the soft solder is coated on the surface to be welded of the porous ceramic, and the wettability of the soft solder on the porous ceramic can be improved due to active elements such as Ti, V and the like, so that the effect of filling and infiltrating the soft solder can be improved.
In some preferred embodiments, the porous ceramic comprises SiCf/SiC, porous Si 3 N 4 Or porous Al 2 O 3 One of them. The materials are easy to obtain.
In some embodiments, the solder paste in step S11 is obtained by mixing solder powder with a third binder. Thus, the mixing effect with the soft solder powder is good.
In some embodiments, the solder powder is selected from Ag-Ti powder, ag-V powder, au-Ti powder, or Cu-Si powder. Thus, the active element in the solder powder can improve wettability of the solder on the porous ceramic.
In some embodiments, the third binder comprises a mixture of terpineol and absolute ethanol, and the volume ratio of terpineol to absolute ethanol is 5 (1-5). Therefore, the mixing effect with soft solder powder is good, and the filling of the follow-up soft solder paste into the gaps of the surface to be welded of the porous ceramic is facilitated.
In some embodiments, before mixing the solder powder with the third binder, further comprising: placing soft solder powder into a ball mill for ball milling, wherein the ball ink process is as follows: and placing the soft solder powder into a ball milling tank to obtain mixed powder, adding absolute ethyl alcohol into the mixed powder, adding grinding balls under the protection of nitrogen, and then performing ball milling.
In some embodiments, the porous ceramic base material and the metal base material need to be mechanically polished by using 80# water sand paper, 400# water sand paper, 800# water sand paper and 1200# water sand paper in sequence to obtain a base material with a smooth surface to be welded; and cleaning the smooth porous ceramic base metal and the metal base metal by using distilled water and acetone respectively, and drying at 40-60 ℃ for 20-40min to obtain the clean surface to be welded after removing impurities.
In some embodiments, in step S12, the heat treatment process includes: heating to 350-450 ℃ at 9-11 ℃/min, preserving heat for 8-10min, volatilizing Yu Song oleyl alcohol, continuing heating to melt the soft solder at 9-11 ℃/min, cooling to 350-450 ℃ at 7-8 ℃/min, and turning off the heating and cooling to room temperature.
In some preferred embodiments, the modified porous ceramic further comprises, prior to step S2: polishing the surface to be welded of the porous ceramic by using No. 2000 sand paper, ultrasonically cleaning the surface with acetone for 8-10min, and drying the surface at the temperature of 40-60 ℃ for 20-40min. Therefore, the clean modified porous ceramic surface to be welded can be obtained, and subsequent welding is facilitated.
In some embodiments, the braze comprises a BNi7 (Ni-Cr- (P)) paste, a TiNi paste, or a TiZrNiCu amorphous foil tape.
In some embodiments, the BNi7 (Ni-Cr- (P)) paste is obtained by mixing a commercial BNi7 (Ni-Cr- (P)) powder with a first binder and the TiNi paste is obtained by mixing a TiNi powder with a second binder. Thereby facilitating subsequent welding.
In some preferred embodiments, the first and second binders comprise a mixture of terpineol and absolute ethanol, and the volume ratio of terpineol to absolute ethanol is 5 (1-5). Therefore, the powder is good in mixing effect with the hard solder powder, and is beneficial to subsequent welding.
The stress relief method in ceramic-metal described in this embodiment has the following advantages over the prior art: the embodiment realizes effective control of the distribution of soft solder and hard solder by a two-step method so as to simultaneously ensure the temperature resistance and the stress release. Specifically, in this embodiment, the soft solder is prefabricated in the gaps of the surface to be welded of the porous ceramic base material, and the soft solder is controlled in the gaps of the ceramic surface instead of the welding layer, so that on one hand, the problem of softening caused by soft metal in high-temperature use can be avoided, and on the other hand, the soft solder in direct contact with the porous ceramic can effectively relieve the residual stress of the joint through plastic deformation. Secondly, the modified porous ceramic base metal and the metal base metal are connected through the hard brazing filler metal with relatively better temperature resistance, so that the modified porous ceramic base metal and the metal base metal are effectively connected, and certain temperature resistance can be ensured.
Example 1
The embodiment provides a stress relieving method in ceramic-metal, which is used for welding SiCf/SiC of silicon carbide fiber reinforced silicon carbide ceramic and metal GH536, and specifically comprises the following steps of:
(1) The soft solder paste is prepared by mixing Ti powder, ag powder and an adhesive according to a certain proportion; the specific proportion is composed of 1-5 parts of Ti powder and 99-95 parts of Ag powder according to mass fraction; wherein the mass ratio of AgTi mixed powder to the adhesive is 1: (0.1-0.2).
The adhesive in the paste solder preparation method is a mixture of terpineol and absolute ethyl alcohol, and the volume ratio of the terpineol to the absolute ethyl alcohol is 5 (1-5).
(2) Sequentially using 80# water sand paper, 400# water sand paper, 800# water sand paper and 1200# water sand paper to mechanically polish SiCf/SiC ceramic, metal base metal and TiZrNiCu amorphous foil strips (35 wt.% Zr,10wt.% Ni,15wt.% Cu and <5wt.% other water sand paper, bal. Ti) to obtain a material with a smooth surface to be welded; carrying out ultrasonic cleaning on the polished material for 15-30 min; drying at 60 ℃ for 40min to obtain the clean surface to be welded after removing impurities.
(3) The soft solder paste prepared in the step (1) is coated on the surface of the SiCf/SiC ceramic base material treated in the step (2) in a screen printing mode, as shown in fig. 2. And (3) feeding the coated SiCf/SiC ceramic parent metal into a vacuum furnace, and carrying out heat treatment according to a certain heating curve. Finally, the surface to be welded of the porous ceramic/AgTi filling layer is polished by No. 2000 sand paper, ultrasonically cleaned by acetone for 10min and dried at 60 ℃ for 40min.
The heating process is that heating to 350 ℃ at 8 ℃/min, preserving heat for 8min to facilitate volatilization of terpineol, then continuing heating to 950-990 ℃ at 8 ℃/min to melt the AgTi cladding layer, then cooling to 350 ℃ at 7 ℃/min, and cooling to room temperature.
(4) Placing the metal base material obtained in the step (2), tiZrNiCu foil tape, and SiCf/SiC ceramic base material treated in the step (3) in order, clamping with a mold at a pressure of about 50g, and feeding into a vacuum furnace (vacuum degree of 5×10) -4 -5×10 -6 Brackets) as shown in fig. 2.
Performing shear strength test on the welding seam of the SiCf/SiC-metal GH536 joint of the silicon carbide fiber reinforced silicon carbide ceramic obtained in the step (4); the shear strength test results showed that the room temperature shear strength of the resulting joint was 69MPa.
And (3) carrying out finite element analysis on the SiCf/SiC-metal GH536 joint of the silicon carbide fiber reinforced silicon carbide ceramic obtained in the step (4). As shown in fig. 3.
Example 2
The embodiment is a comparative example of embodiment 1, and the embodiment provides a method for relieving stress in ceramic-metal, which is used for welding silicon carbide fiber reinforced silicon carbide ceramic SiCf/SiC and metal GH536, and specifically comprises the following steps:
sequentially using 80# water sand paper, 400# water sand paper, 800# water sand paper and 1200# water sand paper to mechanically polish SiCf/SiC ceramic, GH536 metal base metal and TiZrNiCu amorphous foil strips (35 wt.% Zr,10wt.% Ni,15wt.% Cu, 5wt.% other, bal. Ti) to obtain a material with a smooth surface to be welded; carrying out ultrasonic cleaning on the polished material for 15-30 min; drying at 60 ℃ for 40min to obtain the clean surface to be welded after removing impurities.
The metal base material, the TiZrNiCu foil tape and the SiCf/SiC ceramic base material were placed in this order, clamped by a mold, and fed into a vacuum furnace (vacuum degree: 5X 10) -4 -5×10 -6 A bracket).
Finite element analysis was performed on the resulting silicon carbide fiber reinforced silicon carbide ceramic SiCf/SiC-metal GH536 joints. As shown in fig. 4. As can be seen from fig. 3 and 4, the residual stress of the silicon carbide fiber reinforced silicon carbide ceramic SiCf/SiC-metal GH536 joint of the pre-fabricated soft solder in example 1 is smaller than that of the silicon carbide fiber reinforced silicon carbide ceramic SiCf/SiC-metal GH536 joint of the non-pre-fabricated soft solder in example 2.
Example 3
The embodiment provides a stress relief method in ceramic-metal, which is used for welding porous alumina ceramic and TC4, and is specifically completed according to the following steps:
(1) The soft solder paste is prepared by mixing Ti powder, au powder and an adhesive according to a certain proportion; the specific proportion is composed of 1-5 parts of Ti powder and 99-95 parts of Au powder according to mass fraction; wherein the mass ratio of AuTi mixed powder to adhesive is 1: (0.1-0.2).
The hard solder paste is prepared by mixing Ti powder, ni powder and an adhesive according to a certain proportion; the specific proportion is composed of 75-70 parts of Ti powder and 25-30 parts of Ni powder according to mass fraction; wherein the mass ratio of TiNi mixed powder to the adhesive is 1: (0.1-0.2).
The adhesive in the paste solder preparation method is a mixture of terpineol and absolute ethyl alcohol, and the volume ratio of the terpineol to the absolute ethyl alcohol is 5 (1-5).
(2) Sequentially using 80# water sand paper, 400# water sand paper, 800# water sand paper and 1200# water sand paper to mechanically polish the porous alumina ceramic and the TC4 base metal to obtain a base metal with a smooth surface to be welded; carrying out ultrasonic cleaning on the polished material for 15-30 min; drying at 40 ℃ for 20min to obtain the clean surface to be welded after removing impurities.
(3) And (3) coating the coating paste prepared in the step (1) on the surface of the ceramic base material treated in the step (2) in a screen printing mode. And (3) feeding the coated ceramic parent metal into a vacuum furnace, and carrying out heat treatment according to a certain heating curve. Finally, the surface to be welded of the porous ceramic/AuTi cladding layer is polished by No. 2000 sand paper, ultrasonically cleaned by acetone for 10min and dried at 40 ℃ for 40min.
The heating process is that heating to 400 ℃ at 9 ℃/min, preserving heat for 9min to facilitate volatilization of terpineol, then continuing heating to 1000-1050 ℃ at 9 ℃/min to melt the AuTi cladding layer, then cooling to 400 ℃ at 7.5 ℃/min, closing heating, and cooling to room temperature.
(4) Coating the hard solder paste obtained in the step (1) on the surface to be welded of the metal base material obtained in the step two in a screen printing manner, then placing the surface to be welded of the ceramic base material processed in the step three on the surface coated with the metal base material, clamping by a mold, pressing at about 50g, and feeding into a vacuum furnace (vacuum degree is 5×10) -4 ×10 -6 A bracket).
The heating process is that heating to 350 ℃ at 10 ℃/min, preserving heat for 10min to facilitate volatilization of terpineol, then continuing heating to 900-950 ℃ at 10 ℃/min, then cooling to 350 ℃ at 7.5 ℃/min, closing heating, and cooling to room temperature.
Example 4
The embodiment provides a stress relieving method in ceramic-metal, which is used for welding Cf/C composite ceramic and TC4, and is specifically completed according to the following steps:
(1) The soft solder paste is prepared by mixing Si powder, cu powder and an adhesive according to a certain proportion; the specific proportion is composed of 5-10 parts of Si powder and 95-90 parts of Cu powder according to mass fraction; wherein the mass ratio of CuSi mixed powder to adhesive is 1: (0.1-0.2).
The hard solder paste is prepared by mixing commercial BNi7 (Ni-Cr- (P)) and an adhesive according to a certain proportion; wherein the mass ratio of TiNi mixed powder to the adhesive is 1: (0.1-0.2).
The adhesive in the paste solder preparation method is a mixture of terpineol and absolute ethyl alcohol, and the volume ratio of the terpineol to the absolute ethyl alcohol is 5 (1-5).
(2) Sequentially using 80# water sand paper, 400# water sand paper, 800# water sand paper and 1200# water sand paper to mechanically polish the porous alumina ceramic and the TC4 base metal to obtain a base metal with a smooth surface to be welded; carrying out ultrasonic cleaning on the polished material for 30 min; drying at 50deg.C for 30min to obtain clean surface to be welded after removing impurities.
(3) And (3) coating the coating paste prepared in the step (1) on the surface of the ceramic base material treated in the step (2) in a screen printing mode. And (3) feeding the coated ceramic parent metal into a vacuum furnace, and carrying out heat treatment according to a certain heating curve. Finally, the surface to be welded of the porous ceramic/CuSi cladding layer is polished by No. 2000 sand paper, ultrasonically cleaned by acetone for 10min and dried at 50 ℃ for 30min.
The heating process is that heating is carried out at 10 ℃/min to 450 ℃ for 10min to volatilize terpineol, then heating is carried out at 10 ℃/min to 875-900 ℃ to melt the CuSi cladding layer, then heating is carried out at 8 ℃/min to 450 ℃ and then cooling is carried out in a furnace to room temperature (Si reacts with Cf/C parent metal, so that wettability is improved on one hand, component points are offset to Cu on the other hand, the filler in the hole is composed of Cu+SiC phase, and the melting temperature is about 1050 ℃).
(4) Coating the hard solder paste obtained in the step (1) on the surface to be welded of the metal base material obtained in the step (2) in a screen printing manner, then placing the surface to be welded of the ceramic base material processed in the step (3) on the surface coated with the metal base material, clamping by a mold, feeding the mold with a pressure of about 50g into a vacuum furnace (vacuum degree of 5×10) -4 -5×10 -6 A bracket).
The heating process is that heating to 450 ℃ at 10 ℃/min, preserving heat for 10min to facilitate volatilization of terpineol, then continuing heating to 900-975 ℃ at 10 ℃/min, then cooling to 450 ℃ at 7.5 ℃/min, and closing heating, and cooling to room temperature.
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the application.
Claims (6)
1. A method of stress relief in a ceramic-metal comprising:
step S1, coating soft solder on a surface to be welded of a porous ceramic base material, filling the soft solder into a gap of the surface to be welded of the porous ceramic base material to obtain a modified porous ceramic base material filled with the soft solder, wherein the soft solder is obtained by mixing soft solder powder with a third adhesive, and the soft solder powder is selected from Ag-Ti powder, ag-V powder, au-Ti powder or Cu-Si powder;
and S2, coating hard brazing filler metal on the surface of the treated metal base metal, sequentially placing the metal base metal, the hard brazing filler metal and the modified porous ceramic base metal in sequence, clamping by using a die, and sending into a vacuum furnace for heat treatment to finish ceramic-metal connection, wherein the hard brazing filler metal comprises BNi7 paste, tiNi paste or TiZrNiCu amorphous foil strips, and the brazing temperature of the hard brazing filler metal is lower than the melting point of the soft brazing filler metal by 50-200 ℃.
2. The method of claim 1, wherein in step S2, the heat treatment process comprises: heating to 350-450 ℃ at 9-11 ℃/min, preserving heat for 8-10min, continuing heating to the brazing temperature of the hard brazing filler metal at 9-11 ℃/min, preserving heat for 5-15min, melting the hard brazing filler metal, cooling to 350-450 ℃ at 7-8 ℃/min, closing heating, and cooling to room temperature in a furnace.
3. The method of claim 1, wherein the BNi7 paste is obtained by mixing a commercial BNi7 powder with a first binder and the TiNi paste is obtained by mixing a TiNi powder with a second binder.
4. The method for relieving stress in ceramic-metal according to claim 1, wherein in step S1, the coating of solder on the surface to be soldered of the porous ceramic base material comprises:
s11, preparing soft solder paste;
and step S12, coating the soft solder paste on the surface to be welded of the processed porous ceramic base material in a screen printing mode, performing heat treatment in a vacuum furnace, and obtaining the modified porous ceramic base material after post-treatment.
5. The method of claim 1, wherein the third binder comprises a mixture of terpineol and absolute ethanol, and wherein the volume ratio of terpineol to absolute ethanol is 5 (1-5).
6. The method of stress relief in ceramic-metal according to claim 4, wherein in step S12, said heat treatment process comprises: heating to 350-450 ℃ at 9-11 ℃/min, preserving heat for 8-10min, continuing heating to melt the soft solder at 9-11 ℃/min, cooling to 350-450 ℃ at 7-8 ℃/min, and turning off the heating and cooling to room temperature.
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