WO2022193524A1 - Procédé de préparation de plaque de support métallique pour pile à combustible - Google Patents

Procédé de préparation de plaque de support métallique pour pile à combustible Download PDF

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WO2022193524A1
WO2022193524A1 PCT/CN2021/108851 CN2021108851W WO2022193524A1 WO 2022193524 A1 WO2022193524 A1 WO 2022193524A1 CN 2021108851 W CN2021108851 W CN 2021108851W WO 2022193524 A1 WO2022193524 A1 WO 2022193524A1
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sintering
metal
powder
metal substrate
electrolyte
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PCT/CN2021/108851
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English (en)
Chinese (zh)
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包崇玺
陈志东
颜巍巍
童璐佳
朱志荣
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东睦新材料集团股份有限公司
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Publication of WO2022193524A1 publication Critical patent/WO2022193524A1/fr

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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
    • H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
    • 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
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0232—Metals or alloys
    • 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
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0241—Composites
    • 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

Definitions

  • the invention belongs to the technical field of fuel cells, and in particular relates to a preparation method of a metal support plate for fuel cells.
  • Solid oxide fuel cell is an ideal fuel cell, which not only has the advantages of high efficiency and environmental friendliness of fuel cells, but also has the following outstanding advantages:
  • the solid oxide fuel cell is an all-solid structure, and there is no corrosion problem and electrolyte loss caused by the use of a liquid electrolyte, and it is expected to achieve long-life operation.
  • the working temperature of solid oxide fuel cells is 800-1000 °C. Not only does the electrocatalyst not need to use precious metals, but also natural gas, coal gas and hydrocarbons can be directly used as fuels, which simplifies the fuel cell system.
  • the high-temperature waste heat discharged from the solid oxide fuel cell can form a combined cycle with a gas turbine or a steam turbine, which greatly improves the overall power generation efficiency.
  • MS-SOFC metal-supported solid oxide fuel cells
  • SOFC fuel cell supporter SOFC
  • MS-SOFC has its unique advantages: (1) low cost: The cost of metal materials is much lower than that of metal-ceramic composite materials; (2) Fast start-up: The good thermal conductivity of metal can reduce the temperature gradient inside the battery and achieve fast start-up, so that it can be used in the mobile field; (3) Processability: Compared with ceramics, metal materials have better processability, which will greatly reduce the difficulty of SOFC processing; (4) Ease of sealing: The welding and sealing technology of metal materials can avoid the problem of difficult sealing of SOFC.
  • the main function of the metal support is to transport gas, conduct current, and provide stable structural support for the battery.
  • the metal support can be used as an in-situ reforming layer.
  • the hydrocarbon fuel takes the lead in chemical reformation in the metal support, and the generated synthesis gas undergoes electrochemical oxidation in the anode layer.
  • This structure The design can enhance the anode's resistance to carbon deposition and improve the long-term stability of the battery in hydrocarbon fuels.
  • MS-SOFC is not only suitable for traditional solid oxide fuel cell (SOFC) applications, such as stationary power stations, backup power supplies and charging piles, etc., but also as a range extender for mobile devices such as heavy-duty vehicles or electric vehicles.
  • the current metal-supported solid oxide fuel cells such as the Chinese invention patent application "Method for the Preparation of Porous Metal-supported Low-Temperature Solid Oxide Fuel Cells", whose patent application number is CN200610118649.9 (application publication number CN1960047A) discloses a
  • NiO-ScSZ or CGO
  • CGO the raw material of the support body to prepare the support body, and the process is complicated and the manufacturing is difficult.
  • the Fe-Cr alloy support, anode and electrolyte blank prepared by casting are laminated and then sintered at high temperature in a reducing atmosphere.
  • the anode catalyst is injected into the metal support side of the half-cell, and the surface of the electrolyte is screened.
  • the cathode layer was printed, and the anode and cathode were sintered in situ during battery testing. This process effectively avoids the diffusion of metal elements at high temperature.
  • the in-situ sintering temperature is too low, the bonding strength of the interface between the cathode and the electrolyte is low, and the battery performance is attenuated.
  • the porous metal body with anode and electrolyte is prepared by co-casting method.
  • the metal support body and the micro-tubular metal support body are prepared by the dry pressing method. Due to the thin metal support layer, the metal support plate is prone to uneven thickness after dry pressing, resulting in inconsistent sintering deformation and affecting the bonding between the anode, electrolyte, etc. and the substrate; and the metal thickness of the micro-tubular metal support body is not easy to achieve uniform control. , affecting the combination with the anode, etc.
  • Fe-based alloys and Ni-based alloys are used as metal supports for MS-SOFC. Due to the large difference between the thermal expansion coefficient of Ni-based alloys and electrolyte materials, during battery operation, the internal thermal stress is too large, and cracks are likely to occur, and even the electrolyte layer is peeled off. ; The pure Ni support has poor anti-oxidation performance and is easy to agglomerate and coarsen, which makes the SOFC performance attenuate sharply.
  • Ni-based alloys seriously hinder their application in SOFC supports; while Fe-based alloys are used as supports, especially ferritic stainless steel, although ferritic stainless steel has a high temperature thermal expansion coefficient CTE (11 ⁇ 10 -6 ⁇ 13 ⁇ 10 -6 K -1 ) is very close to YSZ (yttria-stabilized zirconia) and GDC (Gd 2 O 3 doped CeO 2 ) (13 ⁇ 10 -6 ⁇ 14 ⁇ 10 -6 K -1 ) electrolytes , but long-term work in a medium-high temperature and humid atmosphere can easily lead to oxidation of metal materials and mutual diffusion of elements between Fe and Cr elements in the stainless steel support and the Ni-based anode.
  • CTE 11 ⁇ 10 -6 ⁇ 13 ⁇ 10 -6 K -1
  • GDC Gd 2 O 3 doped CeO 2
  • the Fe and Cr elements in the support diffuse into the anode, and oxides are formed during the operation of the battery, which leads to the rapid degradation of the battery performance; at the same time, the Ni element in the anode diffuses into the stainless steel support.
  • the thermal expansion coefficient of the support body changes, the internal stress of the battery increases, and the structural stability decreases.
  • the technical problem to be solved by the present invention is to provide a method for preparing a metal support plate for a fuel cell that eliminates sintering deformation and improves the bonding tightness between the anode layer and the substrate in view of the current state of the prior art.
  • the technical solution adopted by the present invention to solve the above-mentioned technical problems is: a method for preparing a metal support plate for a fuel cell, which is characterized in that the following steps are included in sequence:
  • step 2) sieve the powder in step 1), and select the particle size of the powder to be 13-250 ⁇ m;
  • step 2) mixing the powder in step 2) with the forming agent, in terms of mass percentage, the powder accounts for 92-95%, and the forming agent accounts for 5-8%, and after mixing uniformly, a solid metal fluid powder is obtained;
  • step 4) putting the powder in step 3) into a rolling mill for rolling, thereby forming a metal substrate;
  • a sintering treatment is performed between steps 4) and 5) or after step 7).
  • the sintering treatment is to place a metal substrate or a metal support plate of a required size on a setter plate for sintering, the sintering temperature is 1000°C to 1350°C, the sintering time is 5 to 240 minutes, and the vacuum degree is 10 -3 Pa ⁇ 10 2 Pa.
  • the metal support body After sintering, the metal support body has high strength, and the anode and the metal support body are tightly bonded.
  • Co-sintering of anode, electrolyte and cathode can improve production efficiency, reduce production cost, and improve the bonding state of the three interfaces of metal support plate-anode-electrolyte-cathode.
  • the sintered metal substrate is flattened, and then the flattened metal substrate is subjected to a wax dip treatment, that is, a metal substrate of a desired size is placed in the The wax melt is placed in the wax melt for 1 to 30 minutes. After the wax melt penetrates into the pores in the metal substrate, the metal substrate is taken out and cooled. In this way, a relatively flat metal support plate is obtained, and the pores of the metal support plate are reduced by dipping the wax.
  • sintered stainless steel is selected in step 1), and the components of the sintered stainless steel, in terms of mass percentage, include the following components: carbon: ⁇ 0.03%, nickel: 0-25%, molybdenum: 0-4%, chromium: 10 ⁇ 30%, Niobium: 0 ⁇ 3%, Aluminum: 0 ⁇ 10%, Titanium: 0 ⁇ 3%, Silicon: 0 ⁇ 1%, Manganese: 0 ⁇ 2%, unavoidable impurities not exceeding 2%, Iron: surplus.
  • the sintered stainless steel of this composition has a thermal expansion coefficient that matches the anode and electrolyte.
  • the components of the forming agent have various forms, but preferably, the components of the forming agent in step 2), in terms of mass percentage, include the following components: paraffin wax: 40-60%; microcrystalline wax: 20-30% ; Castor oil: 0.5-20%; polyethylene wax: 5-15%; EVA wax: 5-15%; stearic acid: 1-2%.
  • paraffin wax 40-60%
  • microcrystalline wax 20-30%
  • Castor oil 0.5-20%
  • polyethylene wax 5-15%
  • EVA wax 5-15%
  • stearic acid 1-2%.
  • step 5 step 6) and step 7
  • sintering is performed after drying, and the sintering temperature used in the sintering in step 5) and the sintering in step 6) is both 1050 °C ⁇ 1400 °C, sintering
  • the time is 10 ⁇ 300min
  • the sintering temperature used in the sintering in step 7) is 800°C ⁇ 1200°C
  • the sintering time is 5 ⁇ 300min
  • the vacuum degree is 10 -3 Pa ⁇ 10 2 Pa.
  • the metal fiber felt with a porosity greater than 50% is also added to the rolling mill, and the metal fiber felt and the powder are rolled into a metal substrate.
  • the porosity of the metal fiber mat is large, and some metal powder particles will enter the pores of the fiber when rolling, which can change the structure of the fiber.
  • the strength of the sintered fiber mat is high, which can improve the strength of the metal support plate.
  • the component content of the metal fiber felt has various forms, preferably, the metal fiber felt, in terms of mass percentage, includes the following components: carbon: ⁇ 0.06%, nickel: 0-25%, molybdenum: 0-4%, Chromium: 10 to 30%, Niobium: 0 to 3%, Aluminum: 0 to 10%, Titanium: 0 to 3%, Silicon: 0 to 1%, Manganese: 0 to 2%, unavoidable not exceeding 2% Impurities, Iron: Balance.
  • the metal fiber felt of this material is similar to the stainless steel powder material, which is beneficial to improve the strength of the metal support, especially the high temperature strength.
  • the electrolyte slurry includes butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG, glutamic acid PHT, and also includes yttria-stabilized zirconia and LaGaO 3 -based electrolytes , one of Ba(Sr)Ce(Ln)O 3 and CeO 2 -based solid electrolytes.
  • the thermal expansion coefficient of this electrolyte slurry is close to that of the anode and cathode, and the combination is better after sintering.
  • This cathode material is tightly bound to the electrolyte layer.
  • the present invention has the advantages that the preparation method of the metal support plate for the fuel cell is simple in process, can realize mass production of the metal support plate without a mold, reduces the production cost and improves the production efficiency;
  • the sintering deformation is eliminated due to the support of the setter and the sintering shrinkage of the metal support plate is basically close to the anode material, and the bonding tightness between the anode layer and the metal substrate is improved.
  • the powder rolling of the forming agent has higher green strength, controllable sintering shrinkage, and controllable sintering deformation.
  • the density is lower and the weight is lighter, which is conducive to achieving light weight.
  • the support plate prepared from the metal sheet requires multiple coating treatments, which is expensive.
  • the pores of the metal substrate can be controlled to ensure that the gas can easily pass through the metal substrate.
  • 1 is a sectional view of the structure of a metal support plate fuel cell
  • Fig. 2 is the pore morphology after sintering in Example 1;
  • Fig. 3 is the pore morphology after sintering in Example 2.
  • Figure 4 is the pore morphology after sintering in Example 7.
  • Figure 5 is the pore morphology after sintering in Example 8.
  • Figure 6 is the pore morphology after sintering in Example 13;
  • FIG. 7 is the pore morphology after sintering in Example 14.
  • 434L stainless steel powder is selected, and 434L stainless steel powder is calculated by mass percentage, including the following components: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron: balance;
  • step 4) Rolling the green body: place the material in step 3) in the powder rolling hopper, and roll the green body strip, the green body is a metal substrate, the thickness of the strip is 0.55mm, and the width is 130mm.
  • the material is cut into a metal substrate 4 of 110mm ⁇ 110mm ⁇ 0.55mm, and placed on the setter plate;
  • Wax immersion Melt polyethylene wax at 110°C, melting temperature is 119°C, put the metal support plate into the wax melt for 10 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • the metal support plate has many pores, which can ensure good air permeability.
  • the material is 434L stainless steel powder: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron: balance;
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1200°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • Wax immersion Melt polyethylene wax at a melting temperature of 120°C, put the metal support plate into the wax melt for 5 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • the metal support plate has many pores, which can ensure good air permeability.
  • the material is 430L stainless steel powder: C: 0.025%, Cr: 17.1%, Mn: 0.8%, Si: 0.6%, iron: the balance;
  • step 4) Rolling the green body: place the material in step 3) in the powder rolling hopper, roll the green strip, the strip thickness is 0.9mm, the width is 130mm, and the green strip is cut to 110 ⁇ 110 ⁇ 0.9 mm of metal substrate 4 and placed on the setter plate.
  • Sintering The setter on which the powder rolled green body is placed is placed in a push rod furnace for sintering.
  • the sintering temperature is 1250°C, and the sintering time is 30 minutes.
  • the sintering atmosphere used in the sintering process is a mixture of high-purity hydrogen and argon. Mixed gas, in which the volume ratio of argon is 30%.
  • Wax immersion Melt polyethylene wax at a melting temperature of 120°C, put the metal support plate into the wax melt for 5 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • the material is 316L stainless steel powder: C: 0.03%, Cr: 17.8%, Ni: 12.5%, Mn: 1.2%, Si: 0.8%, Mo: 2.48%, iron: balance;
  • step 4) Rolling the green body: place the material in step 3) in the powder rolling hopper, roll the green strip, the strip thickness is 0.9mm, the width is 130mm, and the green strip is cut to 110 ⁇ 110 ⁇ 0.9 mm of metal substrate 4 and placed on the setter plate.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering, the sintering temperature is 1300°C, the sintering time is 30 minutes, and the sintering atmosphere is a mixture of high-purity hydrogen and argon, in which argon The volume ratio is 30%.
  • Wax immersion Melt polyethylene wax at a melting temperature of 120°C, put the metal support plate into the wax melt for 5 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • the materials are iron-chromium-aluminum powder: C: 0.06%, Cr: 21.1%, Mn: 0.9%, Si: 0.3%, Al: 4.79%, iron: balance;
  • step 4) Rolling the green body: place the material in step 3) in the powder rolling hopper, roll the green strip, the strip thickness is 0.9mm, the width is 130mm, and the green strip is cut to 110 ⁇ 110 ⁇ 0.9 mm of metal substrate 4 and placed on the setter plate.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1300°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • Dip wax melt polyethylene wax at a melting temperature of 120°C. Put the metal support plate into the wax melt for 5 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • the material is 310 stainless steel, C: ⁇ 0.25%, Si: ⁇ 1.50%, Mn: ⁇ 2.00%, P: ⁇ 0.045%, S: ⁇ 0.0.03%, Cr: 24.0-26.0%, Ni: 19.0-22.0%, Iron: balance.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1300°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • Dip wax melt polyethylene wax at a melting temperature of 120°C. Put the metal support plate into the wax melt for 5 minutes, and take out the metal plate to cool after the pores have penetrated into the wax.
  • One of paraffin wax, EVA wax or PP wax can also be used.
  • the material is 434L stainless steel powder.
  • the stainless steel powder is calculated by mass percentage, including the following components: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron :margin;
  • step 4) Rolling the green body: place the material in step 3) in the powder rolling hopper, roll the green strip, the strip thickness is 0.9mm, the width is 130mm, and the green strip is cut to 110 ⁇ 110 ⁇ 0.9 mm of metal substrate 4 and placed on the setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Figure 4 shows the pores of the metal support plate. It can be seen that there are many connected pores in the support plate, the density is low, and the porosity is greater than 50%.
  • the support plate of this embodiment is about 50% of the weight of the existing metal support plate with the same thickness, so as to achieve the purpose of light weight.
  • the material is 434L stainless steel powder: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron: balance;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes LaGaO3 - based electrolyte, butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1200°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • Figure 5 shows the pores of the metal support plate. It can be seen that there are many connected pores in the support plate, the density is low, and the porosity is greater than 50%.
  • the support plate of the present invention is about 50% of the weight of the conventional metal support plate of the same thickness, and thus the weight is reduced.
  • the material is 430L stainless steel powder: C: 0.025%, Cr: 17.1%, Mn: 0.8%, Si: 0.6%, iron: the balance;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes Ba(Sr)Ce(Ln)O 3 electrolyte, butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1250°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • the material is 316L stainless steel powder: C: 0.03%, Cr: 17.8%, Ni: 12.5%, Mn: 1.2%, Si: 0.8%, Mo: 2.48%, iron: balance;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 9% ; Stearic acid: 1%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes CeO2 - based solid electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1250°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • the materials are iron-chromium-aluminum powder: C: 0.06%, Cr: 21.1%, Mn: 0.9%, Si: 0.3%, Al: 4.79%, iron: balance;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 9% ; Stearic acid: 1%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • yttria-stabilized zirconia is made into slurry.
  • the electrolyte slurry ingredients include YSZ, NiO, butanone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG, glutamic acid PHT, etc.
  • the prepared slurry is evenly coated on one side of the cut metal substrate 4 by methods such as screen printing or dip coating, and the uncoated side is placed on a setter plate for drying.
  • Electrolyte coating preparation The anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the sintering The plate is dried, whereby the anode layer 2 is formed on the upper surface of the metal substrate 4 .
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1330°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 20%.
  • the material is 310 stainless steel, C: ⁇ 0.25%; Si: ⁇ 1.50%; Mn: ⁇ 2.00%; P: ⁇ 0.045%; S: ⁇ 0.0.03%; Cr: 24.0-26.0%; Ni: 19.0-22.0%, Iron: balance.
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 9% ; Stearic acid: 1%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • step 3 The material of step 3) is placed in the powder rolling hopper, and the green strip is rolled, with a thickness of 0.9 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1300°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 40%.
  • 434L stainless steel powder is selected as the material.
  • 434L stainless steel includes the following components: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron :margin;
  • the metal fiber felt includes the following components: C: 0.015%, Cr: 18.5%, Mn: 0.6%, Si: 0.3%, Ni: 10.1%, iron: balance; the porosity of the metal fiber felt is 80%, and the thickness is 0.1 mm; the material in step 3) and the metal fiber felt are placed in the hopper for powder rolling, and the green strip is rolled together.
  • the thickness of the material is 0.7 mm and the width is 120 mm.
  • the green strip is cut into a metal substrate 4 of 110 ⁇ 110 ⁇ 0.9 mm and placed on the setter.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Figure 6 shows the pores of the metal support plate. It can be seen that there are many connected pores in the support plate, the density is low, and the porosity is greater than 50%.
  • the support plate of the present invention is about 50% of the weight of the conventional metal support plate of the same thickness, and thus the weight is reduced.
  • the material is 430L stainless steel powder.
  • 430L stainless steel includes the following components according to the mass percentage: C: 0.025%, Cr: 17.2%, Mn: 0.9%, Si: 0.5%, iron: balance;
  • the above powder is sieved, and the particle size is selected to be less than 325 meshes, and the bulk density of the powder is 2.25 g/cm 3 .
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the metal fiber felt includes the following components: C: 0.015%, Cr: 17.5%, Mn: 0.6%, Si: 0.3%, Ni: 13.4%, Mo: 2.46%, Iron: balance.
  • the metal fiber felt has a porosity of 60% and a thickness of 1.1 mm; the material in step 3) and the metal fiber felt are placed in a powder rolling hopper, and a green strip is rolled together, with a thickness of 1.6 mm and a width of 130 mm. The green strip was cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • yttria-stabilized zirconia is made into slurry.
  • the electrolyte slurry ingredients include YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • the prepared slurry is evenly coated on one side of the cut metal substrate 4 by methods such as screen printing or dip coating, and the uncoated side is placed on a setter plate for drying.
  • Electrolyte coating preparation yttria-stabilized zirconia (YSZ) is made into slurry. The prepared slurry is uniformly coated on the anode layer by methods such as screen printing or dip coating, and the uncoated side is placed on the setter for drying.
  • YSZ yttria-stabilized zirconia
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1200°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • Figure 7 shows the pores of the metal support plate. It can be seen that there are many connected pores in the support plate, the density is low, and the porosity is greater than 50%.
  • the support plate of the present invention is about 50% of the weight of the conventional metal support plate of the same thickness, and thus the weight is reduced.
  • the material is 434L stainless steel powder.
  • 434L stainless steel includes the following components according to the mass percentage: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron: margin;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 8% ; Stearic acid: 2%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the metal fiber felt includes the following components: C: 0.015%, Cr: 17.2%, Mn: 0.9%, Si: 0.5%, iron: margin.
  • the porosity of the metal fiber felt is 60%, and the thickness is 0.4 mm; the material in step 3) and the metal fiber felt are placed in the hopper for powder rolling, and rolled together to form a green strip with a thickness of 0.8 mm and a width of 130 mm.
  • the green strip is cut into a metal substrate 4 of 110 ⁇ 110 ⁇ 0.9 mm and placed on a setter.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1250°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • the material is 434L stainless steel powder.
  • 434L stainless steel includes the following components in terms of mass percentage: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05%, iron: margin;
  • step 2) Mixing: mix the powder in step 2) with a forming agent, and the components of the forming agent are paraffin wax: 45%; microcrystalline wax: 30%; castor oil: 8%; polyethylene wax: 7%; EVA wax: 9% ; Stearic acid: 1%, mixing ratio: metal powder accounts for 94%, forming agent accounts for 6%, the mixing temperature is above 85 ° C, and the semi-solid metal fluid is obtained after mixing evenly, and the temperature needs to be maintained at 60 ° C ⁇ 80 ° C.
  • the metal fiber felt includes the following components: C: 0.006%, Cr: 21.1%, Mn: 0.9%, Si: 0.3%, Al: 4.79 %, iron: balance; porosity 65%, thickness 0.2mm; place the material and metal fiber felt in step 3) in the hopper for powder rolling, and roll it into a green strip with a thickness of 0.6mm, A width of 130 mm, the green strip was then cut to a metal substrate 4 of 110 x 110 x 0.9 mm and placed on a setter plate.
  • Anode layer preparation the anode slurry is uniformly coated on the upper surface of the cut metal substrate 4 by screen printing or dip coating, and the uncoated lower surface of the metal substrate 4 is placed on the setter plate.
  • the anode layer 2 is formed on the upper surface of the metal substrate 4 by drying.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, methyl ethyl ketone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Electrolyte coating preparation the prepared electrolyte slurry is evenly coated on the anode layer 2 by screen printing or dip coating method, and the uncoated lower surface is placed on a setter plate for drying and sintering, Thus, the electrolyte coating layer 3 is formed on the upper surface of the anode layer 2 .
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, methyl ethyl ketone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • Sintering The setter on which the powder rolled green body is placed is placed in a pusher furnace for sintering.
  • the sintering temperature was 1250°C, and the sintering time was 30 minutes.
  • the sintering atmosphere is a mixed gas of high-purity hydrogen and argon, wherein the volume ratio of argon is 30%.
  • the metal fiber mat is different. Specifically, the metal fiber mat includes the following components in terms of mass percentage: C: 0.006%, Cr: 10%, Mn: 2 %, Si: 1%, Al: 10%, Nb: 2%, Ti: 2%, Ni: 25%, Iron: balance.
  • the heat-resistant steel includes the following components: C: 0.025%, Cr: 30%, Mn: 2%, Mo: 4%, iron: balance.
  • the sintering parameters in step 8) are different, specifically, the sintering temperature is 1050° C., and the sintering time is 300 min.
  • the metal fiber mat is different. Specifically, the metal fiber mat includes the following components in terms of mass percentage: C: 0.006%, Ni: 25%, Cr: 30% %, Mo: 4%, Nb: 3%, Al: 5%, Ti: 3%, Iron: balance.
  • Sintered stainless steel is different. Specifically, sintered stainless steel includes the following components in terms of mass percentage: C: 0.025%, Cr: 10%, Si: 1%, Ni: 25%, Nb: 3%, Al: 10 %, Ti: 3%, Iron: balance.
  • the sintering parameters in step 8) are different, specifically, the sintering temperature is 1400° C., and the sintering time is 10 min.
  • the sintered stainless steel with one of nickel-based alloys, cobalt-based alloys, titanium alloys, and chromium-based alloys.
  • the setter plates of the above embodiments are not easily deformed and cracked during sintering, heating and cooling.

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Abstract

La présente invention concerne un procédé de préparation d'une plaque de support métallique pour une pile à combustible. Le procédé comprend spécifiquement les étapes suivantes : 1) À l'aide d'un acier inoxydable fritté, d'un acier résistant à la chaleur, d'un alliage à base de nickel, d'un alliage à base de cobalt, d'un alliage de titane et d'un alliage à base de chrome ; 2) tamiser la poudre dans l'étape 1) ; 3) mélanger la poudre à l'étape 2) avec un agent de formation, pour obtenir une poudre en tant que fluide métallique semi-solide ; 4) mettre en place la poudre dans l'étape 3) dans un laminoir, et laminer celle-ci pour former un substrat métallique ; 5) revêtir la surface supérieure du substrat métallique avec une bouillie d'anode pour former une couche d'anode sur la surface supérieure du substrat métallique ; 6) revêtir la surface supérieure de la couche d'anode avec une bouillie d'électrolyte pour former un revêtement d'électrolyte sur une surface de la couche d'anode ; et 7) revêtir la surface supérieure du revêtement d'électrolyte avec une bouillie de cathode pour former une couche de cathode sur la surface supérieure du revêtement d'électrolyte, de manière à préparer une plaque de support métallique. La déformation de frittage est éliminée, et l'étanchéité de liaison entre la couche d'anode et le substrat métallique est améliorée.
PCT/CN2021/108851 2021-03-19 2021-07-28 Procédé de préparation de plaque de support métallique pour pile à combustible WO2022193524A1 (fr)

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