CN113245653B - Method for connecting ceramic and metal in air by using solid silver - Google Patents
Method for connecting ceramic and metal in air by using solid silver Download PDFInfo
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- CN113245653B CN113245653B CN202110628940.5A CN202110628940A CN113245653B CN 113245653 B CN113245653 B CN 113245653B CN 202110628940 A CN202110628940 A CN 202110628940A CN 113245653 B CN113245653 B CN 113245653B
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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
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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
- B23K1/20—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
- 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
- B23K1/206—Cleaning
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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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
- B23K2103/52—Ceramics
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- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a method for connecting ceramic and metal in air by using solid silver, belongs to the field of connection of metal and ceramic, and aims to solve the problem that the existing soldered joint of metal/ceramic is poor in high-temperature reduction resistance and oxidation resistance. The brazing connection method comprises the following steps: firstly, pressing silver powder into silver sheets; secondly, polishing and cleaning the ceramic to be welded and the metal to be welded; thirdly, stacking the cleaned metal to be welded, the silver sheet and the cleaned ceramic to be welded in sequence, and applying brazing pressure; and fourthly, placing the assembled piece to be welded in a muffle furnace, performing brazing connection at the brazing temperature of 860-960 ℃ for 20-60 min, and cooling to room temperature to complete the brazing connection of the ceramic and the metal. According to the invention, pure silver is used for connecting metal and ceramic, no dispersed oxide exists in the joint, the oxide layer on the metal side is thinner, the high-temperature oxidation resistance and the reduction resistance of the joint are enhanced, and the welding temperature is relatively lower.
Description
Technical Field
The invention relates to the field of connection of metal and ceramic, in particular to a method for connecting ceramic and metal in air by using solid silver.
Background
The solid fuel cell is a clean and efficient electrochemical energy conversion system and is widely applied in various fields. Higher voltages are typically achieved by stacking a plurality of cells in series, which require stainless steel connectors in close proximity to the ceramic electrolyte and thus separate the oxidizing gas (air or O)2) With fuel gas (H)2、CHxCO, etc.). The solid fuel cell is usually used at 600-.
Air reaction brazing is the most common method for joining a metal support to a ceramic cell sheet, and is carried out in air, using silver-oxide as a brazing material, and improving the wetting of silver on the surface of the base material by an oxide (usually CuO) to obtain a dense brazed joint. However, this approach has several disadvantages: firstly, CuO is reduced in the service process, holes are formed in the joint, and the reduction resistance of the joint is reduced; secondly, CuO can aggravate the oxidation of a metal side (usually ferrite stainless steel) to form a thicker oxide layer, so that the oxidation resistance of the joint is reduced; thirdly, the brazing temperature is high (usually higher than 960 ℃), which leads to severe oxidation of the metal base material. And if the brazing filler metal is not added with CuO, the wettability of the brazing filler metal is poor, and the joint defects are more. Therefore, it is necessary to develop a novel method which can not only obtain a compact joint, but also make the joint have strong reduction resistance and oxidation resistance at high temperature.
Disclosure of Invention
The invention provides a method for connecting ceramic and metal in air by using solid silver, aiming at solving the problem that the existing metal/ceramic soldered joint has poor high-temperature anti-reduction and oxidation resistance.
The method for connecting the ceramic and the metal in the air by using the solid silver is realized according to the following steps:
firstly, pressing silver powder into silver sheets;
secondly, polishing the surface to be welded of the metal to be welded by using sand paper, polishing the ceramic to be welded by using a diamond grinding disc, and then putting the ceramic to be welded into absolute ethyl alcohol for ultrasonic cleaning to obtain the cleaned ceramic to be welded and the metal to be welded;
thirdly, stacking the cleaned metal to be welded, the silver sheet and the cleaned ceramic to be welded in sequence, and applying brazing pressure to obtain an assembled part to be welded;
and fourthly, placing the assembled piece to be welded in a muffle furnace, performing brazing connection at the brazing temperature of 860-960 ℃ for 20-60 min, and cooling to room temperature to complete the brazing connection of the ceramic and the metal.
The invention provides a method for connecting ceramic and metal in air by using solid silver. Because the silver has good plasticity and can be remarkably softened at 860-960 ℃, the gap between the silver and the parent metal can be fully filled under the assistance of the assembling pressure, and the close contact between the silver and the parent metal is realized. After heat preservation, silver atoms can diffuse into the parent metal to realize bonding among atoms, thereby forming reliable connection. Pure silver is not reduced and does not promote oxidation of the metal side. The use of pure silver for bonding a metal to a ceramic at a temperature not higher than the melting point (961.8 ℃) of silver does not require consideration of the wettability of silver, and can significantly reduce the diffusion of an element on the metal side into the ceramic.
The method for connecting the ceramic and the metal in the air by using the solid silver mainly comprises the following beneficial effects:
1. the pure silver is used for connecting the metal and the ceramic, no dispersed oxide exists in the joint, and the oxide layer on the metal side is thinner, so that the high-temperature oxidation resistance and the reduction resistance of the joint are enhanced.
2. Silver is solid in the welding process, and a compact joint can be obtained without considering the wettability of the silver on the surface of the base metal.
3. The diffusion rate of the element in solid silver is lower than that of liquid silver, and the diffusion of the element on the metal side to the ceramic can be obviously reduced.
4. The welding temperature is relatively low, and the oxidation of metal in the welding process can be reduced.
Drawings
FIG. 1 is a back-scattering photograph of the microstructure of AISI 441 stainless steel/YSZ ceramic joint obtained at 920 deg.C/30 min/2MPa using 100 μm silver plate in example one;
FIG. 2 is an enlarged view of the stainless steel side of the AISI 441 stainless steel/YSZ ceramic joint obtained at 920 deg.C/30 min/2MPa using 100 μm silver flakes in example one;
FIG. 3 is a back scattering photograph of the microstructure of AISI 441 stainless steel/YSZ ceramic joint subjected to an oxidation test at 800 ℃/300h, obtained under the conditions of 920 ℃/30min/2MPa by using a 100 μm silver plate in example one;
FIG. 4 is an enlarged view of the stainless steel side of the AISI 441 stainless steel/YSZ ceramic joint obtained by using 100 μm silver plate under 920 deg.C/30 min/2MPa in the first example after the 800 deg.C/300 h oxidation test;
FIG. 5 is a back scattering photograph of the microstructure of the AISI 441 stainless steel/YSZ ceramic joint subjected to the 800 ℃/300h reduction test, obtained under the conditions of 920 ℃/30min/2MPa by using a 100 μm silver plate in example one;
FIG. 6 is an enlarged view of the stainless steel side of the AISI 441 stainless steel/YSZ ceramic joint obtained by using 100 μm silver plate under 920 deg.C/30 min/2MPa after 800 deg.C/300 h reduction test in example one;
FIG. 7 is an enlarged view of YSZ ceramics obtained after AISI 441 stainless steel/YSZ ceramic joints obtained by using 100 μm silver sheets under the conditions of 920 ℃/30min/2MPa are subjected to 800 ℃/300h reduction tests in the first example.
Detailed Description
The first embodiment is as follows: the method for connecting the ceramic and the metal in the air by using the solid silver is implemented according to the following steps:
firstly, pressing silver powder into silver sheets;
secondly, polishing the surface to be welded of the metal to be welded by using sand paper, polishing the ceramic to be welded by using a diamond grinding disc, and then putting the ceramic to be welded into absolute ethyl alcohol for ultrasonic cleaning to obtain the cleaned ceramic to be welded and the metal to be welded;
thirdly, stacking the cleaned metal to be welded, the silver sheet and the cleaned ceramic to be welded in sequence, and applying brazing pressure to obtain an assembled part to be welded;
and fourthly, placing the assembled piece to be welded in a muffle furnace, performing brazing connection at the brazing temperature of 860-960 ℃ for 20-60 min, and cooling to room temperature to complete connection of the ceramic and the metal.
The embodiment uses pure silver to connect metal and ceramic below the melting point of silver (961.8 ℃), and the obtained joint has the following beneficial effects: firstly, pure silver cannot be reduced, oxidation of the metal side cannot be aggravated, and the joint has strong reduction resistance and oxidation resistance; secondly, silver is not melted, and the wettability of the silver on the surface of the parent metal does not need to be considered; thirdly, the brazing temperature is low, so that the oxidation degree of the surface of the base material can be reduced; and fourthly, compared with liquid silver, the solid silver can obviously reduce the diffusion of elements on the metal side to the ceramic.
The second embodiment is as follows: this embodiment is different from the first embodiment in that the silver powder is pressed using a tablet press in the first step.
The third concrete implementation mode: the present embodiment is different from the first or second embodiment in that the silver powder in the first step has a particle size of 1 to 20 μm.
The fourth concrete implementation mode: the present embodiment is different from the first to third embodiments in that the silver sheet in the first step has a thickness of 100 to 500 μm.
The fifth concrete implementation mode: the difference between the embodiment and one of the first to the fourth embodiments is that in the second step, the surfaces to be welded of the metals to be welded are sequentially ground by 200#, 600#, 1000# sandpapers, and the ceramics to be welded are sequentially ground by 600#, 1000# diamond grinding discs.
The sixth specific implementation mode: the difference between the embodiment and one of the first to fifth embodiments is that the metal to be welded in the second step is AISI 310S stainless steel, AISI 441 stainless steel, Inconel 600 nickel alloy or Crofer 22APU stainless steel.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is that the ceramic to be welded in the second step is YSZ ceramic or Al2O3Ceramics, ZTA ceramics, SiO2Ceramic, SiC ceramic or perovskite ceramic (GDC ceramic, LSCF ceramic, BSCF ceramic, BCFN ceramic, BZCY ceramic or bzcyb ceramic).
The specific implementation mode is eight: the difference between the present embodiment and one of the first to seventh embodiments is that the brazing pressure applied in the third step is 0.1 to 5 MPa.
The specific implementation method nine: the present embodiment is different from the first to eighth embodiments in that the temperature raising speed is controlled to be 2 to 10 ℃/min in the fourth step.
The detailed implementation mode is ten: the difference between the present embodiment and one of the first to ninth embodiments is that in the fourth step, the brazing connection is performed under the conditions that the brazing temperature is 880-930 ℃ and the heat preservation time is 25-40 min.
The first embodiment is as follows: the method for connecting the ceramic and the metal in the air by using the solid silver is implemented according to the following steps:
firstly, pressing silver powder with the particle size of about 10 mu m into silver tablets with the thickness of 100 mu m by using a tablet press;
secondly, sequentially polishing the surfaces to be welded of the AISI 441 stainless steel by using 200#, 600#, 1000# abrasive paper, sequentially polishing the YSZ ceramics by using 600#, 1000# diamond millstones, and then putting the YSZ ceramics into absolute ethyl alcohol for ultrasonic cleaning treatment to obtain cleaned ceramics to be welded and metals to be welded;
thirdly, stacking the cleaned metal to be welded, the silver sheet and the cleaned ceramic to be welded in sequence, and applying brazing pressure of 2MPa to obtain an assembled part to be welded;
fourthly, placing the assembled piece to be welded in a muffle furnace, controlling the heating speed to be 10 ℃/min, carrying out brazing connection under the conditions of the brazing temperature of 920 ℃ and the heat preservation time to be 30min, and then cooling to the room temperature at the cooling speed of 5 ℃/min to complete the connection of the ceramic and the metal.
The shear strength of the ceramic-to-metal joint obtained in this example was about 86.1 MPa.
The back-scattering photograph of the microstructure of the AISI 441 stainless steel/YSZ ceramic joint obtained in this example using a 100 μm silver plate at 920 deg.C/30 min/2MPa is shown in FIG. 1.
As can be seen from fig. 1 and 2, the joint obtained by the method of the present invention has only silver in the weld, no other products, no reactive layer on the ceramic side of YSZ and a thin oxide layer (about 2 μm) on the surface of stainless steel, whereas conventional air reaction brazing forms an oxide layer over 20 μm on the surface of stainless steel.
From fig. 3 and 4, it can be seen that the reaction layer on the surface of the stainless steel becomes thicker after 300h of oxidation, but remains dense, providing good airtightness to the joint. The oxidation of the joint is much lower than that obtained using air reaction brazing. Wherein the oxidation test is as follows: the welded joint was placed in a tube furnace and compressed air was passed through the tube furnace at a flow rate of 6L/h and held at 800 ℃ for 300 h.
Through 5, 6 and 7, the joint still keeps compact after being reduced for 300h, no obvious change is found on the ceramic side and the metal side, and the phenomenon that CuO is reduced is avoided. Wherein the reduction test: placing the welded joint into a tube furnace, and adding Ar-5% H2The temperature was maintained at 800 ℃ for 300h by passing through a tube furnace at a flow rate of 6L/h.
Claims (10)
1. Method for connecting ceramic and metal in air using solid silver, characterized in that the method for connecting ceramic and metal is carried out according to the following steps:
firstly, pressing silver powder into silver sheets;
secondly, polishing the surface to be welded of the metal to be welded by using sand paper, polishing the ceramic to be welded by using a diamond grinding disc, and then putting the ceramic to be welded into absolute ethyl alcohol for ultrasonic cleaning to obtain the cleaned ceramic to be welded and the metal to be welded;
thirdly, stacking the cleaned metal to be welded, the silver sheet and the cleaned ceramic to be welded in sequence, and applying brazing pressure to obtain an assembled part to be welded;
and fourthly, placing the assembled piece to be welded in a muffle furnace, performing brazing connection at the brazing temperature of 860-960 ℃ for 20-60 min, and cooling to room temperature to complete the brazing connection of the ceramic and the metal.
2. The method for connecting ceramics and metals in the air using solid silver according to claim 1, characterized in that the silver powder is compressed using a tablet press in the first step.
3. The method for connecting ceramics and metals in the air using solid silver according to claim 1, wherein the particle size of the silver powder in the first step is 1 to 20 μm.
4. The method for connecting ceramics and metals in the air by using solid silver according to claim 1, wherein the thickness of the silver plate in the first step is 100 to 500 μm.
5. The method for connecting ceramics and metals in the air by using solid silver according to claim 1, wherein in the second step, the surfaces to be welded of the metals to be welded are sequentially ground by 200#, 600#, 1000# sandpaper, and the ceramics to be welded are sequentially ground by 600#, 1000# diamond grinding discs.
6. The method for connecting ceramics and metals in the air using solid silver according to claim 1, characterized in that the metal to be welded in step two is AISI 310S stainless steel, AISI 441 stainless steel, Inconel 600 nickel alloy or Crofer 22APU stainless steel.
7. The method for connecting ceramics and metals in the air by using solid silver as claimed in claim 1, wherein the ceramics to be welded in the second step is YSZ ceramics, Al2O3Ceramics, ZTA ceramics, SiO2Ceramic, SiC ceramic or perovskite ceramic.
8. The method for connecting ceramics and metals in the air by using solid silver according to claim 1, wherein the brazing pressure applied in the third step is 0.1 to 5 MPa.
9. The method for connecting ceramics and metals in the air by using solid silver according to claim 1, wherein the temperature rise rate in the fourth step is controlled to be 2-10 ℃/min.
10. The method for connecting the ceramic and the metal in the air by using the solid silver according to claim 1, wherein the brazing connection is performed in the fourth step under the conditions that the brazing temperature is 880-930 ℃ and the heat preservation time is 25-40 min.
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