CN114426435B - Direct diffusion bonding method for ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel - Google Patents
Direct diffusion bonding method for ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel Download PDFInfo
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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
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
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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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/40—Metallic
- C04B2237/408—Noble metals, e.g. palladium, platina or silver
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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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention relates to a direct diffusion bonding method of ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel, which comprises the following steps: gradually polishing the surfaces to be connected of the ternary layered ceramics and the ferritic stainless steel by using metallographic abrasive paper, and then polishing by using diamond grinding paste; mixing Ti 3 SiC 2 The ceramics are arranged in contact with the large surface of SUS430 stainless steel, a temperature measurement platinum wire is welded on the side surface of the sample, and the welded sample is subjected to diffusion connection; and after the connection experiment is finished, cooling and removing pressure to obtain the diffusion connection joint. The joint obtained by the method provided by the invention has good interface combination, low connection temperature, good service performance and mechanical property, a continuous reaction layer is generated on the interface, and no obvious welding defects such as cracks, air holes and the like exist, so that the problem of Cr volatilization of an alloy connector can be solved, the preparation and processing costs of a ceramic connector are reduced, and the ternary layered ceramic Ti is expanded 3 SiC 2 And the application range of the solid solution material thereof.
Description
Technical Field
The invention belongs to the technical field of ceramic connection and solid oxide fuel cell connectors, and particularly relates to a direct diffusion connection method of ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel.
Background
Solid Oxide Fuel Cells (SOFC) belong to the third generation of Fuel cells, and are all Solid state chemical power generation devices that directly convert chemical energy stored in Fuel and oxidant into electrical energy at medium and high temperatures with high efficiency and environmental friendliness. The connector is one of the key parts of the plate type solid oxide fuel cell SOFC stack, and is used for electrically connecting the cell units and separating and distributing fuel gas of an anode and oxidizing gas of a cathode.
Titanium silicon carbide (Ti) 3 SiC 2 ) The ceramic material is a novel ternary laminar machinable ceramic material, is a member of MAX phase ceramic family, wherein M refers to transition metal, A refers to main group metal, and X refers to C or N element. Ti 3 SiC 2 Combines the advantages of ceramics and metals, such as low density, high modulus, high strength, high thermal conductivity, good oxidation resistance, easy processing and the like. Thus Ti 3 SiC 2 The ceramic has wide application prospect in the high-tech fields of aviation, aerospace, nuclear industry, electronic information and the like, is a novel structure-function integrated material, and is particularly suitable to be used as a connector material of a solid oxide fuel cell. In particular, for Ti 3 SiC 2 Optimized for doping (Ti, M) 3 SiC 2 The (M = Nb, W, ta, V) material is oxidized to generate (Ti, M) O in the service environment of SOFC 2 And amorphous SiO 2 The conductivity and the oxidation resistance of the uniformly mixed single-layer oxide film are compared with the Cr with the same thickness 2 O 3 Is high. At the same time, the user can select the desired position,(Ti,M) 3 SiC 2 the material has excellent electric and thermal conductivity, high strength, high creep resistance and proper thermal expansion coefficient, and is a very potential material for SOFC connectors. However, ti 3 SiC 2 The finished product rate of the solid solution material is low, the processing and manufacturing cost is high, and certain difficulty exists in synthesizing block materials or components with large size or complex shape, so that Ti is limited 3 SiC 2 For large-scale applications.
The ferritic stainless steel containing Cr is a key point for application and research of connector materials due to the advantages of low price, excellent corrosion resistance, oxidation resistance, oxide film conductivity, thermal expansion coefficient similar to other components and the like. The alloy forms compact Cr with good conductivity on the surface 2 O 3 The layer protects the substrate. However, in the long-term operation of SOFC (600-800 ℃), cr is on the cathode side 2 O 3 Easy to form Cr 6+ Volatile matter (Cr) 2 O 3 Or CrO 2 (OH) 2 ) The activity of the cathode material is reduced, so that the cathode is poisoned, and the failure process of the galvanic pile is accelerated. Therefore, solving the poison of Cr volatilization of an alloy connector to a cathode is an important guarantee for maintaining the long-term stable work of the SOFC galvanic pile.
Aiming at the problem of Cr volatilization, at present, two solutions are mainly adopted at home and abroad, firstly, a novel low-Cr alloy is developed, so that a double-layer structure oxide film is generated on the surface of the alloy after the alloy is oxidized, and the outer layer is non-Cr 2 O 3 Layer, inner layer being continuous Cr 2 O 3 Layer, outer layer compact non-Cr 2 O 3 The layer can act as a barrier to the volatilization of Cr compounds to some extent, but the problem of volatilization still remains, and further improvement of the long-term properties of the interconnect is still needed. Another solution is to prepare a protective coating on the surface of the alloy, but the long-term stability of the coating remains to be investigated.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a direct diffusion bonding method of ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel, wherein Ti is used for bonding Ti, titanium silicon carbon and ferritic stainless steel in a diffusion mode 3 SiC 2 Welding ceramic and ferritic stainless steel，Ti 3 SiC 2 The ceramic or its solid solution is placed on the cathode side to solve the problem of chromium volatilization, and the ferritic stainless steel is placed on the anode side to reduce Ti 3 SiC 2 The using amount of the ceramics further reduces the preparation and processing expenses, and finally the purpose of providing a solid oxide fuel cell connector material which has low cost, complex manufacturing shape and excellent performance is achieved, and the material is applied to the field of solid oxide fuel cell connectors; meanwhile, the welding connection technology can improve the reliability of the ceramic structure and can be used for repairing damaged ceramic pieces. Therefore, the method not only has high theoretical significance, but also has very important practical value.
The technical scheme of the invention is as follows:
a diffusion bonding method of ternary laminated ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel comprises the following specific steps:
the method comprises the following steps: sample to be joined of ternary laminated ceramic and ferritic stainless steel (10 x 2mm) 3 Block) surfaces are respectively polished by metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000# and then polished by diamond grinding paste; then ultrasonically cleaning and drying for later use;
step two: 10 x 10mm of the sample treated in step one 2 The flat surfaces are arranged in contact and then are arranged in 10 x 2mm of ternary laminated ceramic and ferritic stainless steel 2 Welding a platinum wire on the side surface, placing a sample for welding the platinum wire in a vacuum chamber of a thermal simulation testing machine, wherein the vacuum degree of the equal cavity is 5 multiplied by 10 -3 Heating is started when Pa, the heating rate is set to be 10 ℃/min, the temperature is increased to 900-1200 ℃, the pressure is 5-30 MPa, the pressure increasing rate is 1MPa/min, the heat preservation time is 30-150 min, and the sample is subjected to diffusion connection; the welded platinum wire is used as a temperature control platinum wire;
step three: after the connection experiment is finished, the thermal simulation testing machine is cooled to the room temperature at the cooling rate of 10 ℃/min under the original vacuum condition, then pressure is removed at a constant speed, and the pressure is 0 when the temperature is reduced to the room temperature, so that the diffusion connection joint is obtained.
Further, the ternary layered ceramic comprises titanium silicon carbon and solid solution thereof, and the solid solution is prepared by adding titanium silicon carbon and titanium silicon carbonThe titanium silicon carbon doped modified solid solution has the molecular formula of (Ti, M) 3 SiC 2 ，M＝Nb,Ta,W,V。
Further, the ferritic stainless steel is an alloy interconnect material commonly used for solid oxide fuel cells, and the ferritic stainless steel is any one of SUS430, SS430, fe-10Cr, 1.4724, fe-17Cr-0.2Y, 1.4016, ferrotherm (1.4742), fe-18Cr-9W, fe-20Cr-7W, fe-20Cr, AL 453, 1.4763 (446), feCrMn (LaTi), fe-Cr-Mn, fe-25Cr-DIN 50049, fe-25Cr-0.1Y-2.5Ti, fe-25Cr-0.2Y-1.6Mn, fe-25Cr-0.4La, fe-25Cr-0.3Zr, fe26CrTiY, fe26CrTiNbY, fe26CrMoTiY, E-Brite, al29-4C, and Fe-30 Cr.
Further, in the first step, before the surface treatment, the ternary layered ceramic and the ferritic stainless steel are cut into 10 × 2mm respectively 3 Sample size of (2).
Further, the pressure in the second step is 5-30 MPa, and the heat preservation time is 30-150 min, preferably 30min, 60min and 90min.
Further, the pressure in the third step is a unidirectional pressure, and the loading direction of the unidirectional pressure is perpendicular to the connecting surface.
The experiment adopts a thermal simulation testing machine Gleeble3000, and can also select a diffusion bonding experiment in a hot pressing furnace.
The invention has the beneficial effects that:
in order to obtain a complete diffusion connection joint with good service performance and mechanical property, the invention utilizes the solid phase diffusion connection technology to realize ternary layered ceramic Ti 3 SiC 2 And the solid solution material thereof is connected with the ferritic stainless steel; the joint interface obtained by the method has good combination, the connection temperature is lower relative to soldering and the like, after the joint is connected by the method provided by the invention, the interface generates a continuous reaction layer without welding defects such as obvious large cracks, air holes and the like, and the prepared SOFC connector material has excellent oxidation resistance and low surface specific resistance, and enlarges the ternary layered ceramic Ti 3 SiC 2 And the application range of the solid solution material has high practical value.
Drawings
FIG. 1 is a schematic diagram of a sample for diffusion bonding according to the present invention;
fig. 2 is a photograph of an interface backscattered electron image after connection according to example 1 of the present invention.
In fig. 1, ferritic stainless steel; 2. titanium silicon carbon and solid solutions thereof; 3. and measuring the temperature of the platinum wire.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
For a further understanding of the present invention, reference will now be made in detail to the present invention with reference to the following examples.
Example 1
Mixing Ti 3 SiC 2 The ceramic and SUS430 stainless steel were cut into 10 × 2mm pieces, respectively 3 Size of Ti, then adding Ti 3 SiC 2 The surfaces to be connected of the ceramic and SUS430 stainless steel are gradually polished by metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000#, and then polished by diamond grinding paste with the granularity of 1 mu m; then ultrasonically cleaning and drying for later use. Placing the material subjected to surface treatment into a pre-treatment machine, and placing Ti on a horizontal table 3 SiC 2 10X 10mm of ceramic and SUS430 stainless steel 2 Arranged by contacting the surfaces, and then welding at Ti 3 SiC 2 Platinum wires were welded to the 2mm side edges of the ceramic and SUS430 stainless steel metal blocks. Fixing the welded sample in a vacuum chamber of a thermal simulation testing machine, and when the vacuum degree reaches 5 multiplied by 10 -3 Heating at Pa, maintaining at 1000 deg.C and 20MPa for 30min, and diffusion bonding with Ti 3 SiC 2 Ceramics and SUS430 stainless steel. After the connection is finished, the thermal simulation testing machine is cooled to the room temperature at the speed of 10 ℃/min under the original vacuum condition, then the vacuumizing is stopped, and the pressure is removed at a constant speed. By scanning electron microscopeAnd observing the microscopic appearance of the connected interface, wherein the interface connection is good, and no obvious air holes, cracks or residual welding lines exist.
Example 2
Mixing Ti 3 SiC 2 The ceramic and SUS430 stainless steel were cut into 10 × 2mm pieces, respectively 3 Size of Ti, then adding Ti 3 SiC 2 The surfaces to be connected of the ceramic and SUS430 stainless steel are gradually polished by metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000#, and then polished by diamond grinding paste with the granularity of 1 mu m; then ultrasonically cleaning and drying for later use. Placing the material subjected to surface treatment into a pre-treatment machine, and placing Ti on a horizontal table 3 SiC 2 10X 10mm of ceramic and SUS430 stainless steel 2 The surfaces are arranged in contact with each other and then welded to Ti by a welding gun 3 SiC 2 Platinum wires were welded to the 2mm side edges of the ceramic and SUS430 stainless steel metal blocks. Fixing the welded sample in a vacuum chamber of a thermal simulation testing machine, and when the vacuum degree reaches 5 multiplied by 10 -3 Heating at Pa, maintaining at 1150 deg.C and 10MPa for 60min, and diffusion bonding with Ti 3 SiC 2 Ceramics and SUS430 stainless steel. After the connection is finished, the thermal simulation testing machine is cooled to the room temperature at the speed of 10 ℃/min under the original vacuum condition, then the vacuumizing is stopped, the pressure is removed at a constant speed, and the pressure is removed to 0 after the temperature is reduced to the room temperature. The microscopic appearance of the interface after the connection is observed by a scanning electron microscope, the interface connection is good, and no obvious air holes, cracks or residual welding lines exist.
Example 3
Mixing Ti 3 SiC 2 The ceramic and Crofer22APU stainless steel are cut into 10X 2mm by wire cutting 3 Size of Ti, then adding Ti 3 SiC 2 The surfaces to be connected of the ceramics and the Crofer22APU stainless steel are gradually polished by metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000#, then polished by diamond grinding paste with the granularity of 1 mu m, and then ultrasonically cleaned and dried for later use. Placing the material subjected to surface treatment into a pre-treatment machine, and placing Ti on a horizontal table 3 SiC 2 10X 10mm of ceramic and SUS430 stainless steel 2 The surfaces are arranged in contact with each other and then welded to Ti by a welding gun 3 SiC 2 Platinum wires are welded on the 2mm side edges of the ceramic and Crofer22APU stainless steel metal blocks. Fixing the welded sample in a vacuum chamber of a thermal simulation testing machine, and when the vacuum degree reaches 5 multiplied by 10 -3 Heating at Pa, maintaining at 1200 deg.C and 10MPa for 30min, and diffusion bonding with Ti 3 SiC 2 Ceramic and Crofer22APU stainless steel. After the connection is finished, the thermal simulation testing machine is cooled to the room temperature at the speed of 10 ℃/min under the original vacuum condition, then the vacuumizing is stopped, the pressure is removed at a constant speed, and the pressure is removed to 0 after the temperature is reduced to the room temperature. The microscopic appearance of the connected interface is observed by a scanning electron microscope, the interface connection is good, and no obvious pores, cracks or residual welding lines exist.
Example 4
Mixing Ti 3 SiC 2 Cutting ceramic and Fe-18Cr-9W stainless steel into 10 × 2mm 3 Size of Ti, then adding Ti 3 SiC 2 The surfaces to be connected of the ceramic and the Fe-18Cr-9W stainless steel are gradually polished by metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000#, then polished by diamond grinding paste with the granularity of 1 mu m, and then ultrasonically cleaned and dried for later use. Placing the material subjected to surface treatment into a pre-treatment machine, and placing Ti on a horizontal table 3 SiC 2 10X 10mm of ceramic and SUS430 stainless steel 2 The surfaces are arranged in contact with each other and then welded to Ti by a welding gun 3 SiC 2 Platinum wires are welded on the side edges of 2mm of the ceramic and Fe-18Cr-9W stainless steel metal blocks. Fixing the welded sample in a vacuum chamber of a thermal simulation testing machine, and when the vacuum degree reaches 5 multiplied by 10 -3 Heating at Pa, maintaining at 900 deg.C and 30MPa for 90min, and diffusion bonding Ti 3 SiC 2 Ceramics and Fe-18Cr-9W stainless steel. After the connection is finished, the thermal simulation testing machine is cooled to the room temperature at the speed of 10 ℃/min under the original vacuum condition, then the vacuumizing is stopped, the pressure is removed at a constant speed, and the pressure is removed to 0 after the temperature is reduced to the room temperature. And the microscopic appearance of the connected interface is observed by a scanning electron microscope, the interface connection is good, and no obvious air holes, cracks or residual welding lines exist.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (3)
1. A direct diffusion bonding method of ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel is characterized by comprising the following specific steps:
the method comprises the following steps: the surfaces to be connected of the ternary layered ceramics and the ferritic stainless steel are respectively polished step by using metallographic abrasive paper of 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000#, and then polished by using diamond grinding paste; then ultrasonically cleaning and drying for later use;
step two: arranging the large plane surface of the sample material treated in the step one in a contact way, welding a temperature measuring platinum wire on the side surfaces of the ternary laminated ceramic and the ferritic stainless steel, placing the sample welded with the platinum wire in a vacuum chamber of a thermal simulation testing machine, and setting the vacuum degree to be 5 multiplied by 10 -3 Heating is started when Pa, the heating rate is set to be 10 ℃/min, the temperature is increased to 900-1200 ℃, the pressure is 5-30 MPa, the pressure increasing rate is 1MPa/min, the heat preservation time is 30-150 min, and the sample is subjected to diffusion connection;
step three: after the connection experiment is finished, cooling the thermal simulation testing machine to room temperature at a cooling rate of 10 ℃/min under the original vacuum condition, then removing pressure at a constant speed, and when the temperature is reduced to the room temperature, making the pressure be 0 to obtain a diffusion connection joint;
the ternary layered ceramic comprises titanium silicon carbon and a solid solution thereof, wherein the solid solution is a titanium silicon carbon doped modified solid solution with a molecular formula of (Ti, M) 3 SiC 2 ，M＝Nb,Ta,W,V；
The ferritic stainless steel is any one of SUS430, crofer22APU and Fe-18 Cr-9W.
2. The method according to claim 1, wherein in the first step, the ternary layered ceramic and the ferrite are first treated before the surface treatment is performedCutting stainless steel into 10 × 2mm 3 Sample size of (2).
3. The method of claim 1, wherein the pressure in step two is a unidirectional pressure, and the unidirectional pressure is loaded in a direction perpendicular to the connecting surface.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273155A (en) * | 2013-05-10 | 2013-09-04 | 山东大学 | Diffusion bonding method of silicon carbide ceramics and ferritic stainless steel |
| CN106851871A (en) * | 2017-01-13 | 2017-06-13 | 杭州格拉思康科技有限公司 | Ceramic layered heating |
| CN107540401A (en) * | 2016-12-26 | 2018-01-05 | 安徽工业大学 | A kind of diffusion connection method of ternary layered ceramic titanium carbon silicide and crome metal |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273155A (en) * | 2013-05-10 | 2013-09-04 | 山东大学 | Diffusion bonding method of silicon carbide ceramics and ferritic stainless steel |
| CN107540401A (en) * | 2016-12-26 | 2018-01-05 | 安徽工业大学 | A kind of diffusion connection method of ternary layered ceramic titanium carbon silicide and crome metal |
| CN106851871A (en) * | 2017-01-13 | 2017-06-13 | 杭州格拉思康科技有限公司 | Ceramic layered heating |
Non-Patent Citations (1)
| Title |
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| Ti3SiC2 陶瓷/Fe扩散连接接头强度及断裂行为;尹孝辉等;《热加工工艺》;20190430;第48卷(第7期);第19-22页 * |
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