WO2023087446A1 - Procédé de fabrication de plaque de support métallique pour pile à combustible - Google Patents

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

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WO2023087446A1
WO2023087446A1 PCT/CN2021/137655 CN2021137655W WO2023087446A1 WO 2023087446 A1 WO2023087446 A1 WO 2023087446A1 CN 2021137655 W CN2021137655 W CN 2021137655W WO 2023087446 A1 WO2023087446 A1 WO 2023087446A1
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Prior art keywords
sintering
metal
powder
metal substrate
stainless steel
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PCT/CN2021/137655
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English (en)
Chinese (zh)
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包崇玺
陈志东
颜巍巍
童璐佳
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东睦新材料集团股份有限公司
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Publication of WO2023087446A1 publication Critical patent/WO2023087446A1/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
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention belongs to the technical field of fuel cells, and in particular relates to a method for manufacturing a metal support plate used in fuel cells.
  • the solid oxide fuel cell is an ideal fuel cell, which not only has the advantages of high efficiency and environmental friendliness of the fuel cell, but also has the following outstanding advantages: (1) The solid oxide fuel cell is an all-solid structure, and there is no liquid electrolyte band Corrosion problems and electrolyte loss problems in the future are expected to achieve long-life operation. (2) The operating temperature of the solid oxide fuel cell is 800-1000°C. Not only does the electrocatalyst not need to use noble metals, but it can also directly use natural gas, coal gas and hydrocarbons as fuel, which simplifies the fuel cell system. (3) Solid oxide fuel cells discharge high-temperature waste heat and can form a combined cycle with gas turbines or steam turbines to greatly improve the total power generation efficiency.
  • the current metal-supported solid oxide fuel cell is such as the Chinese invention patent application "A Method for Manufacturing a Metal Support Plate for Fuel Cells" previously applied by the applicant, whose patent application number is CN202110297120.2 (application publication number CN113054215A) discloses a method for preparing a metal support plate for a fuel cell, which includes the following steps in turn: 1) using sintered stainless steel, heat-resistant steel, nickel-based alloy, cobalt-based alloy, titanium alloy, chromium-based alloy 2) sieve the powder in step 1), and choose a powder particle size of 13-250um; 3) place the powder in the inner hole of the measuring device, remove excess powder, and place it on the setter; 4 ) sintering the setter with measuring device; 5) coating the anode slurry on the upper surface of the metal substrate to form an anode layer on the upper surface of the metal substrate; 6) coating the electrolyte slurry on the anode 7) coating the cathode slurry on the upper surface of the
  • the technical problem to be solved by the present invention is to provide a method for manufacturing a metal support plate used in a fuel cell, so that the strength of the prepared metal support plate is high.
  • the technical solution adopted by the present invention to solve the above-mentioned technical problems is: a method for manufacturing a metal support plate for a fuel cell, which is characterized in that it includes the following steps in sequence: 1) using metal powder and having a mesh number of 20 mesh to 1000 Purpose wire mesh, the material of the wire mesh is deformed superalloy or stainless steel;
  • step 2) Sieving the metal powder in step 1), and selecting the powder particle size to be 10-500 ⁇ m;
  • At least one set of wire mesh and metal powder is placed, and in each group, the wire mesh and metal powder are arranged from bottom to top;
  • sintering sintering the setter plate with the measuring device to obtain a sintered body of the metal substrate
  • the stainless steel is one of austenitic stainless steel, ferritic stainless steel and heat-resistant stainless steel.
  • the metal powder is one of stainless steel, heat-resistant steel, nickel-based alloy, cobalt-based alloy, titanium alloy, and chromium-based alloy.
  • the metal substrate is placed on a setter for sintering, the sintering temperature is 1000°C-1500°C, the sintering time is 5-240min, and the vacuum degree is 10 -3 Pa-10 2 Pa.
  • the metal support body has high strength, and at the same time, the anode and the metal support body are closely combined.
  • the co-sintering of the anode, electrolyte and cathode can improve production efficiency, reduce production costs, and improve the bonding state of the three interfaces of the metal support plate-anode-electrolyte-cathode.
  • sintering is carried out after drying in step 7), step 8) and step 9), the sintering temperatures used in the sintering in step 7) and the sintering in step 8) are all 1050°C to 1400°C, and the sintering The time is 10-300 min.
  • the sintering temperature used in step 9) is 800°C-1200°C, the sintering time is 5-300 min, and the vacuum degree is 10 -3 Pa-10 2 Pa.
  • wax immersion treatment is performed between step 5) and step 6) or between step 6) and step 7), that is, the metal substrate is placed in the wax melt for 1-30 minutes, and the pores in the metal substrate are After infiltration into the wax melt, the metal substrate is removed and allowed to cool. In this way, a relatively flat metal support plate is obtained, and the pores of the metal support plate are reduced by wax dipping treatment.
  • the metal powder is stainless steel powder.
  • the stainless steel powder includes the following components: carbon: ⁇ 0.03%, nickel: 0-25%, molybdenum: 0-4%, chromium: 10-30% %, silicon: 0-1%, manganese: 0-2%, unavoidable impurities not exceeding 2%, iron: the balance.
  • Stainless steel with this composition has a thermal expansion coefficient that matches that of the anode, electrolyte, etc.
  • the superalloy includes the following components in terms of mass percentage: C: 0-0.15%, Cr: 14-35%, Mo: 0-10%, W: 0-16%, Al: 0-2.2% %, Ti: 0 to 3.0%, Fe: 0 to 5%, unavoidable impurities: less than 2%, nickel: the balance.
  • the electrolyte slurry includes butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG, glutamic acid PHT, and also includes yttria-stabilized zirconia, LaGaO3- based electrolyte , Ba(Sr)Ce(Ln)O 3 and CeO 2 based solid electrolytes.
  • the coefficient of thermal expansion 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 bonded to the electrolyte layer.
  • the present invention has the advantages that: the metal support plate adopts a metal connecting plate containing metal mesh and metal powder, the sintering shrinkage is small, and the sintered steel-steel material is formed after co-sintering, which has high strength and can be used
  • the metal powder adjusts the pore diameter of the wire mesh, which is beneficial for the gas participating in the fuel cell reaction to pass through the metal support plate.
  • the metal mesh is used to strengthen the sintered metal, and the strength is more than 20% higher than that of the sintered metal with the same porosity.
  • the preparation method of the above-mentioned metal support plate has a simple process, can realize mass production of the metal support plate without a mold, reduces production cost, and improves production efficiency.
  • Figure 1 is a cross-sectional view of the metal support plate fuel cell structure
  • Fig. 2 is the pore morphology of wire mesh in embodiment 1;
  • Fig. 3 is the morphology of wire mesh and stainless steel powder co-sintering in embodiment 1;
  • Fig. 4 is the pore morphology of one side of the wire mesh after sintering in embodiment 1;
  • Fig. 5 is the pore morphology of the cross section of the sintered wire mesh and stainless steel powder in Example 1.
  • the metal powder is 434L stainless steel powder.
  • the 434L stainless steel powder includes the following components: C: 0.025%, Cr: 17.5%, Mn: 0.8%, Si: 0.6%, Mo: 1.05 %, Fe balance and unavoidable impurities no more than 2%; the metal mesh adopts 700 mesh 304 stainless steel wire mesh with a size of 120 ⁇ 120mm, and the pore morphology of the stainless steel wire mesh is shown in Figure 2;
  • step 3 Put the wire mesh in step 1) into the bottom of the inner hole of the measuring device, then pour the powder in step 2) into the measuring device to remove excess powder; 1.2mm;
  • the setter is ceramics containing 95% alumina, and the setter with the measuring device in step 3) is sintered at a sintering temperature of 1250°C and a sintering time of 120min, and the vacuum degree is kept at 10- 3 Pa to 10 2 Pa, in order to prevent chromium volatilization, the sintering atmosphere is vacuum backfilled with 3 ⁇ 10 4 Pa argon, and the sintered billet is taken out after sintering;
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, butanone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT;
  • the electrolyte slurry includes yttria-stabilized zirconia YSZ electrolyte, butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT;
  • Fig. 3 is the morphology of wire mesh and stainless steel powder co-sintering in embodiment 1;
  • Fig. 4 is the pore morphology of the wire mesh side after sintering in embodiment 1;
  • Fig. 5 is the pore morphology after sintering in embodiment 1 The pore morphology of the cross-section after sintering of wire mesh and stainless steel powder. It can be seen from Figure 3 to Figure 5 that good sintering necks are formed between the powder particles, between the powder and the screen, and between the wires of the screen, so that the strength of the metal support plate is improved.
  • the tensile strength of the metal support plate at room temperature after sintering is 116 MPa, and the flatness of the support plate is 0.25 mm.
  • the tensile strength of metal powder using the same material as in this embodiment is not more than 70MPa, and the flatness is above 0.5mm. Therefore, the tensile strength of the metal support plate prepared in this embodiment is higher.
  • the difference between this embodiment and the above-mentioned embodiment 1 is only that the metal powder and wire mesh used are different, specifically, the metal powder is 316L stainless steel powder.
  • the 316L stainless steel powder includes the following components: C: 0.025%, Cr: 17.3%, Mn: 1.1%, Si: 0.7%, Mo: 2.55%; the metal mesh adopts 500-mesh 434 stainless steel wire mesh;
  • step 2) the particle size range of the sieved metal powder is 100 mesh to 150 mesh (106 to 150 ⁇ m), and the bulk density of the powder is 2.55 g/cm 3 ;
  • the sintering temperature for sintering in step 4) is 1230° C., the sintering time is 30 minutes, and the sintering atmosphere is 80% hydrogen+20% argon;
  • step 5 the height of the sintered compact is pressed to 0.75mm, and the density after pressing is 4.7g/cm 3 ;
  • Wax immersion treatment is carried out between step 5) and step 6), immersing the sintered body in the paraffin melt for 3 minutes, taking it out and scraping off excess paraffin above the plane of the metal substrate.
  • the aforementioned anode slurry includes yttria-stabilized zirconia YSZ, NiO, butanone, ethanol, triethanolamine, starch, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • the aforementioned electrolyte slurry includes yttria-stabilized zirconia electrolyte, butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • the tensile strength of the metal support plate at room temperature after sintering in this embodiment is 128MPa, and the flatness of the support plate is 0.30mm.
  • the tensile strength of metal powder using the same material as in this embodiment is not more than 70MPa, and the flatness is above 0.45mm. Therefore, the tensile strength of the metal support plate prepared in this embodiment is higher.
  • the selected metal powder and wire mesh are different.
  • the metal powder is 430L stainless steel powder.
  • the 430L stainless steel powder includes the following components: C: 0.021%, Cr: 17.1%, Mn: 0.7%, Si: 0.4%; the metal mesh adopts 600-mesh FeCrAl heat-resistant steel wire mesh;
  • step 2) the particle size range of the sieved metal powder is 200 mesh to 250 mesh, and the bulk density of the powder is 2.25g/cm 3 ;
  • step 3 a wire mesh is placed in the measuring vessel, followed by the above-mentioned metal powder. After the height of the metal powder is 0.6mm, the wire mesh and the metal powder are alternately placed in turn. This time, the height of the metal powder is 1.2mm. remove excess powder;
  • the sintering temperature for sintering in step 4) is 1260° C., the sintering time is 30 minutes, and the sintering atmosphere is 100% hydrogen;
  • Wax immersion treatment is carried out between step 5) and step 6), immersing the sintered body in the paraffin melt for 3 minutes, taking it out and scraping off excess paraffin above the plane of the metal substrate.
  • the aforementioned electrolyte slurry includes CeO 2 -based solid electrolyte, butanone, ethanol, triethanolamine, polyvinyl butyral PVB, polyethylene glycol PEG and glutamic acid PHT.
  • the metal substrate in this embodiment has high tensile strength.
  • the metal powder and wire mesh used are different.
  • the metal powder is GH1140 powder.
  • the GH1140 powder heat-resistant steel powder
  • the wire mesh is 500 mesh FeCrAl heat-resistant steel wire mesh
  • step 2) the particle size range of the sieved metal powder is 150 mesh to 200 mesh, and the bulk density of the powder is 2.35g/cm 3 ;
  • step 3 a wire mesh is placed in the measuring vessel, and then the above-mentioned metal powder is placed, and the height of the metal powder is 1.2 mm to remove excess powder;
  • the sintering temperature for sintering in step 4) is 1290° C., the sintering time is 60 minutes, and the sintering atmosphere is 100% hydrogen;
  • step 5 the height of the sintered compact is pressed to 0.75mm, and the density after pressing is 4.85g/cm 3 ;
  • Wax immersion treatment is carried out between step 5) and step 6), immersing the sintered body in the paraffin melt for 3 minutes, taking it out and scraping off excess paraffin above the plane of the metal substrate.
  • 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.
  • the metal substrate in this embodiment has high tensile strength.
  • the selected metal powder is different from the wire mesh, specifically, the selected metal powder is different from the wire mesh, specifically, the metal powder is GH4033 powder (nickel-based alloy powder ), according to mass percentage, the GH4033 powder includes the following components: C: 0.05%, Cr: 21.21%, Mn: 0.35%, Si: 0.35%, Fe: 3.5%, Al: 0.95%, Ti: 2.7% , Ni: balance; wire mesh, using 325 mesh FeCrAl heat-resistant steel wire mesh;
  • step 2) the particle size range of the sieved metal powder is 325 mesh to 400 mesh, and the bulk density of the powder is 2.15g/cm 3 ;
  • step 3 a wire mesh is placed in the measuring vessel, and then the above-mentioned metal powder is placed, and the height of the metal powder is 1.2 mm to remove excess powder;
  • the sintering temperature for sintering in step 4) is 1310° C., the sintering time is 80 minutes, and the sintering atmosphere is 100% hydrogen;
  • step 5 the height of the sintered compact is pressed to 0.75mm, and the density after pressing is 4.55g/cm 3 ;
  • Wax immersion treatment is carried out between step 5) and step 6), immersing the sintered body in the paraffin melt for 3 minutes, taking it out and scraping off excess paraffin above the plane of the metal substrate.
  • the metal substrate in this embodiment has high tensile strength.
  • Embodiment 6 is a diagrammatic representation of Embodiment 6
  • the metal powder is 430L stainless steel powder
  • the stainless steel powder includes the following components in terms of mass percentage: carbon: 0.02%, nickel: 12%, molybdenum: 4%, chromium : 10%, manganese: 2%, unavoidable impurities not exceeding 2%, iron: balance.
  • the sintering temperature for sintering in step 4) is 1000°C, and the sintering time is 240min;
  • the flattening in step 5) adopts rolling machine to carry out rolling, and the thickness after rolling is 0.65mm;
  • step 7), step 8) and step 9), sintering is carried out after drying, the sintering temperature adopted in the sintering in step 7) and the sintering in step 8) are all 1050° C., and the sintering time is 10 min.
  • the sintering temperature in 9) is 800° C., the sintering time is 5 minutes, and the vacuum degree is 10 ⁇ 3 Pa.
  • Embodiment 7 is a diagrammatic representation of Embodiment 7:
  • the metal powder is 430L stainless steel powder
  • the stainless steel powder includes the following components in terms of mass percentage: carbon: 0.01%, nickel: 25%, molybdenum: 4%, chromium : 30%, silicon: 1%, unavoidable impurities not exceeding 2%, iron: the balance.
  • the wire mesh adopts 20-mesh superalloy (GH4037) wire mesh, and the superalloy wire mesh includes the following components according to the mass ratio: C: 0.07%, Cr: 21%, Mo: 3%, W: 6%, Al: 2.2%, Ti: 2.5%, Fe: 5%, unavoidable impurities: less than 2%, nickel: balance.
  • the sintering temperature in step 4) is 1500° C., and the sintering time is 5 minutes; in order to prevent elements such as chromium from evaporating, 5 ⁇ 10 4 Pa of argon can be backfilled.
  • step 7), step 8) and step 9), sintering is carried out after drying, the sintering temperature adopted in the sintering in step 7) and the sintering in step 8) are all 1400°C, and the sintering time is 300min.
  • the sintering temperature in 9) is 1200° C.
  • the sintering time is 300 min
  • the vacuum degree is 10 2 Pa.
  • Embodiment 8 is a diagrammatic representation of Embodiment 8
  • the superalloy wire mesh of this example adopts (GH4033) in terms of mass percentage, including the following components: C: 0.06%, Cr: 20%, Al: 0.7%, Ti : 2.6%, Fe: 2%, unavoidable impurities: less than 2%, nickel: balance.
  • the aforementioned superalloy is 1000 mesh.
  • the metal powder is one of nickel-based alloy, cobalt-based alloy, titanium alloy and chromium-based alloy.
  • step 7 in step 7), step 8) and step 9) all carry out sintering after drying, the sintering in step 7) and the sintering in step 8) adopt the sintering
  • the temperature is 1200° C., and the sintering time is 50 minutes.
  • the sintering temperature used in step 9) is 900° C., the sintering time is 60 minutes, and the vacuum degree is 10 2 Pa.
  • step 3 at least two groups of wire mesh and metal powder can be placed in the measuring vessel, and the two groups are arranged in sequence from bottom to top (that is, the wire mesh and metal powder are alternately placed from bottom to top), and in each group
  • the wire mesh can be made of the same material or different materials to remove excess powder.
  • Embodiment 9 is a diagrammatic representation of Embodiment 9:
  • the superalloy wire mesh of this example includes the following components in terms of mass percentage: C: 0.15%, Cr: 14%, W: 16%, Al: 0.7% , Ti: 3.0%, Fe: 2%, unavoidable impurities: less than 2%, nickel: balance.
  • the aforementioned superalloy is 1000 mesh.
  • Metal powder adopts cobalt-based alloy.
  • the superalloy wire mesh of this example includes the following components in terms of mass percentage: C: 0.15%, Cr: 35%, Mo: 10%, Al: 0.7% , Ti: 3.0%, Fe: 5%, unavoidable impurities: less than 2%, nickel: balance.
  • the aforementioned superalloy is 1000 mesh.
  • the metal powder is one of nickel-based alloy, cobalt-based alloy, titanium alloy and chromium-based alloy.
  • the powder measuring device is designed according to the size of the metal support plate and the sintering shrinkage rate.
  • the shape of the inner hole of the measuring device is preferably larger than the target size of the support plate.
  • Measuring instruments usually adopt through-hole measuring instruments and bottom measuring instruments.
  • the wire mesh and the metal powder are alternately placed in the through-hole measuring device in turn.
  • the wire mesh layer has 1 to 100 layers, and the powder higher than the powder measuring device is removed with a scraper. Take out the powder measure. After each metal powder is put in, push it flat and then place the wire mesh.
  • the wire mesh layer has 1 to 100 layers. Put it into the measuring device, and finally cover the setter plate on the top of the powder measuring device containing powder, turn over 180° together with the setter plate and the measuring device, and take out the powder measuring device.
  • the above-mentioned wire mesh and metal powder are alternately arranged, and the mesh materials and mesh numbers of different layers may be the same or different.

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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

L'invention concerne un procédé de fabrication d'une plaque de support métallique pour une pile à combustible, lequel procédé comprend les étapes successives suivantes : 1) adopter une poudre métallique et un treillis métallique, le treillis métallique étant fait d'un superalliage corroyé ou d'un acier inoxydable ; 2) cribler la poudre métallique dans l'étape 1), la taille des particules de la poudre sélectionnée étant de 10 à 500 µm ; 3) placer au moins un groupe de treillis métalliques et la poudre métallique, dans chaque groupe, les treillis métalliques et la poudre métallique étant agencés de bas en haut ; 4) fritter ; 5) aplatir ; 6) couper ; 7) former une couche d'anode sur la surface supérieure d'un substrat métallique ; 8) former un revêtement d'électrolyte sur la surface supérieure de la couche d'anode ; et 9) former une couche de cathode sur la surface supérieure du revêtement d'électrolyte, et ainsi préparer la plaque de support métallique. Une plaque de liaison métallique contenant un filet métallique et une poudre métallique est utilisée, de telle sorte que le retrait de frittage est faible, un matériau acier-acier fritté est formé après frittage, et une résistance élevée est obtenue.
PCT/CN2021/137655 2021-11-22 2021-12-14 Procédé de fabrication de plaque de support métallique pour pile à combustible WO2023087446A1 (fr)

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CN202111388849.7A CN114142046A (zh) 2021-11-22 2021-11-22 用于燃料电池的金属支撑板的制造方法
CN202111388849.7 2021-11-22

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CN102903945A (zh) * 2012-10-26 2013-01-30 中国科学院上海硅酸盐研究所 一种制备大尺寸平板式金属支撑型固体氧化物燃料电池的方法
CN113054215A (zh) * 2021-03-19 2021-06-29 东睦新材料集团股份有限公司 一种用于燃料电池的金属支撑板的制造方法
CN113067005A (zh) * 2021-03-19 2021-07-02 东睦新材料集团股份有限公司 一种用于燃料电池的金属支撑板的制备方法

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