WO2020017796A1 - Procédé de fabrication d'une pile à combustible à oxyde solide permettant d'empêcher une dégradation sous une tension de cellule négative - Google Patents

Procédé de fabrication d'une pile à combustible à oxyde solide permettant d'empêcher une dégradation sous une tension de cellule négative Download PDF

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WO2020017796A1
WO2020017796A1 PCT/KR2019/008198 KR2019008198W WO2020017796A1 WO 2020017796 A1 WO2020017796 A1 WO 2020017796A1 KR 2019008198 W KR2019008198 W KR 2019008198W WO 2020017796 A1 WO2020017796 A1 WO 2020017796A1
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layer
solid oxide
oxide fuel
fuel cell
electrolyte
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Korean (ko)
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임형태
손민지
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창원대학교 산학협력단
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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
    • 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
    • H01M4/8605—Porous electrodes
    • H01M4/8621—Porous electrodes containing only metallic or ceramic material, e.g. made by sintering or sputtering
    • 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
    • H01M4/8636—Inert electrodes with catalytic activity, e.g. for fuel cells with a gradient in another property than porosity
    • H01M4/8642—Gradient in composition
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • H01M4/8885—Sintering or firing
    • H01M4/8889—Cosintering or cofiring of a catalytic active layer with another type of layer
    • 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
    • H01M4/90—Selection of catalytic material
    • 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
    • H01M4/90—Selection of catalytic material
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9033—Complex oxides, optionally doped, of the type M1MeO3, M1 being an alkaline earth metal or a rare earth, Me being a metal, e.g. perovskites
    • 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
    • H01M8/0236—Glass; Ceramics; Cermets
    • 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
    • H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
    • 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
    • H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
    • H01M8/1226—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material characterised by the supporting layer
    • 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
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • 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
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
    • H01M8/1253—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing zirconium oxide
    • 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
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/241—Grouping of fuel cells, e.g. stacking of fuel cells with solid or matrix-supported electrolytes
    • H01M8/2425—High-temperature cells with solid electrolytes
    • 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
    • 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 present invention is (i) Ministry of Trade, Industry and Energy's national research and development project (project unique number: 20163030031850, business name: energy technology development project, research project name: development of high reliability SOFC stack manufacturing technology for distributed generation, research management professional organization: energy technology Assessment Agency, Organizer: Mico Corporation, Research Period: 2017.10.01 ⁇ 2018.07.30) and (ii) National R & D project implemented by Ministry of Science and Technology Information and Communication (Project number: 2017M1A2A2045018, Project name: climate change technology development project, Project Title: Development of in-situ diagnostic technology for optimizing SOFC stack design, Research and management agency: Korea Research Foundation, Organized by Changwon National University Industry-University Cooperation Group, Research Period: 2018.05.01 ⁇ 2019.02.28) As a result of Changwon University,
  • the present invention relates to a method for manufacturing a solid oxide fuel cell, and more particularly, to a method for manufacturing a solid oxide fuel cell including an electrolyte layer having a structure capable of preventing degradation of an SOFC cell stack under a negative cell voltage. It is about.
  • the electromotive force of a fuel cell is about 1V maximum per unit cell, and stacking several cells in series is necessary to obtain a desired output.
  • the low performing cell operates at a negative cell voltage above the threshold current value, causing physical destruction due to rapid deterioration, thereby stopping the entire stack operation. (FIG. 1).
  • This phenomenon is a phenomenon commonly occurring in electrochemical devices connected in series. In order to stabilize and commercialize a battery, performance deviation between cells must be minimized.
  • YSZ zirconia
  • the oxygen ion conductivity is different depending on the point of view.
  • pure oxygen ion conductivity has the advantage of high open circuit voltage and therefore high power.
  • pure oxygen ion conductivity no longer serves as an advantage.
  • Korean Patent No. 10-1180182 (a solid oxide fuel cell with excellent peeling resistance) uses a triple layer electrolyte to include a ceria component only in an electrolyte layer close to an anode to impart electronic conductivity, thereby providing leakage current. And deterioration to the reverse voltage was suppressed.
  • a multilayer electrolyte structure has several drawbacks, such as complicated manufacturing process, high resistance due to thick electrolyte, and interfacial resistance between layers.
  • the technical problem to be solved by the present invention is a solid oxide that can effectively prevent the separation between the negative electrode layer and the electrolyte layer in a reverse voltage situation without generating problems such as the complexity and resistance of the electrolyte layer manufacturing process of the prior art It is to provide a fuel cell manufacturing method.
  • the cell using the YSZ electrolyte not only reduces the voltage per hour, but also the open circuit voltage and power density after operation. After the analysis, it was found that exfoliation was observed at the interface between the anode and the electrolyte.
  • YSZ Yttria-stabilized zirconia
  • the cause of the peeling phenomenon between the negative electrode and the electrolyte interface is due to the high oxygen partial pressure at the negative electrode / electrolyte interface due to the reverse voltage. It is important to reduce the oxygen partial pressure at the interface to prevent the peeling phenomenon.
  • the present invention is a method of not directly adding ceria to the inside of an electrolyte, and forms a negative electrode layer containing ceria having electronic conductivity on one surface during cell manufacturing, and sinters the cell to obtain a high temperature.
  • the present invention (a) an anode layer having a layer containing ceria (CeO 2 ) formed on one surface; An electrolyte layer formed on the layer including ceria and including Yttria-stabilized zirconia (YSZ); And manufacturing a solid oxide fuel cell unit cell stacked in the order of the cathode layer. And (b) sintering the solid oxide fuel cell unit cell, wherein the reverse voltage degradation phenomenon is prevented.
  • the negative electrode layer is an anode functional layer (Anode Functional Layer,) formed on the negative electrode support layer as a layer comprising an anode support (AS) and the ceria AFL).
  • the negative electrode support layer and the negative electrode functional layer may be made of a nickel (Ni) -based material, and further, the negative electrode support layer may include nickel and YSZ, and the negative electrode functional layer may include nickel, YSZ and ceria.
  • the anode layer may include a cathode functional layer (CFL) formed on the electrolyte layer and a cathode collector layer (Current Collector, CC) formed on the anode functional layer.
  • CFL cathode functional layer
  • CC cathode collector layer
  • the positive electrode functional layer may include SSM (Sr-doped LaMnO 3 ) and YSZ
  • the positive electrode current collector layer may include an LSM.
  • step (b) the unit cell prepared in step (a) is sintered, and the cerium ions are diffused into the electrolyte layer from the layer containing ceria provided on the cathode side through sintering.
  • a gradient structure in which the cerium concentration decreases toward the center of the electrolyte layer from the electrolyte layer interface is formed.
  • the sintering conditions in the step (b) is a sintering temperature and time if the inclined structure of a predetermined thickness (but should be smaller than the total thickness of the electrolyte layer) from the cathode layer and the electrolyte layer interface can be formed Is not particularly limited, and may be, for example, 1 to 11 hours at a temperature of 1410 to 1510 °C.
  • a solid oxide fuel cell stack including a plurality of unit cells is provided.
  • a solid oxide fuel cell (SOFC) according to the present invention
  • cerium ions are diffused from the layer containing ceria provided on the cathode side into the electrolyte layer from the cathode / electrolyte layer interface.
  • a solid oxide fuel cell having a gradient anode / electrolyte structure in which cerium concentration decreases toward the center of the electrolyte layer may be manufactured, and the solid oxide fuel cell may locally have only an electrolyte section close to the cathode / electrolyte interface. It has an electron conductivity (N-type) to effectively prevent the negative electrode / electrolyte peeling in the reverse voltage situation, and since only a part of the inside of the electrolyte has an electronic conductivity it can also prevent the leakage current.
  • N-type electron conductivity
  • the cerium ions are diffused into a single layer of an electrolyte layer through a sintering process to locally provide electronic conductivity to the inside of the electrolyte layer, thereby eliminating the need for forming a multilayer electrolyte structure requiring a complicated manufacturing process as in the prior art. It is possible to manufacture a solid oxide fuel cell which can ensure durability against voltage and also prevent leakage current.
  • I-V current-voltage
  • FIG. 2 is a flowchart illustrating each step of a method of manufacturing a solid oxide fuel cell in which reverse voltage degradation is prevented according to the present invention.
  • FIG. 3 is a flow chart illustrating each step of the SOFC cell manufacturing process having a gradient anode / electrolyte structure according to an embodiment of the present invention.
  • FIG. 4 is a schematic cross-sectional view of an SOFC cell having a gradient anode / electrolyte structure manufactured according to an embodiment of the present disclosure.
  • FIG. 6 (a) is a graph showing a voltage change with time when a constant current (CC) is applied to a conventional SOFC cell including a YSZ electrolyte layer
  • FIG. 6 (b) is a graph showing a measurement result of a corresponding constant current test IV
  • 6 (c) is a scanning electron microscope (SEM) photograph showing the cell cross-sectional microstructure after the constant current test.
  • FIG. 7 (a) is a graph showing the voltage change over time when applying a constant current (CC) for the SOFC cell manufactured in the present embodiment
  • Figure 7 (b) is a graph showing the result of the constant current test IV measurement
  • FIG. 7 (c) is a scanning electron microscope (SEM) photograph showing the cell cross-sectional microstructure after the constant current test.
  • Embodiments according to the concepts of the present invention may be variously modified and may have various forms, and specific embodiments will be illustrated in the drawings and described in detail in the present specification or application. However, this is not intended to limit the embodiments in accordance with the concept of the present invention to a particular disclosed form, it should be understood to include all changes, equivalents, and substitutes included in the spirit and scope of the present invention.
  • steps (1) to (6) below were sequentially performed to fabricate an SOFC unit cell having a gradient anode / electrolyte structure having a cross-sectional schematic diagram shown in FIG. 4.
  • NiO, YSZ, and ceria were mixed at a ratio of 60 wt%: 20 wt%: 20 wt%, respectively, for the production of the anode functional layer (AFL), and further grinding was performed using a planetary ball mill to refine the particles.
  • the anode functional layer mixed with LSM and YSZ was screen printed on the sintered cell and heat-treated at 1170 °C for 1 hour.
  • Anode made of LSM was screen printed on the anode functional layer and heat-treated at 1160 ° C for 1 hour.
  • EDS analysis was performed to analyze how the ceria diffused into the electrolyte during sintering of the unit cell prepared in the above example.
  • FIG. 5 which shows the results of EDS analysis, it was found that cerium diffused about 3 microns in a 15 micron thick electrolyte. Through this, it can be seen that a region having a local electron conductivity exists inside the YSZ electrolyte.
  • the cell to which the gradient anode / electrolyte manufactured in the present embodiment is applied maintains the voltage under high voltage and low voltage as well as in reverse voltage (FIG. 7 (a)).
  • the performance is also not significantly different from the existing YSZ cell (Fig. 7 (b)), and the post analysis showed that no physical damage occurs between the anode and the electrolyte interface (Fig. 7 (c)).
  • the cerium ions are diffused into the electrolyte layer from the layer containing ceria provided on the cathode side through a high temperature sintering process.
  • a solid oxide fuel cell having a gradient anode / electrolyte structure in which cerium concentration decreases from the electrolyte layer interface toward the center of the electrolyte layer may be manufactured, and the solid oxide fuel cell may have an electrolyte close to the cathode / electrolyte interface.
  • the cerium ions are diffused into the single layer of the electrolyte layer through the sintering process to locally supply the electronic conductivity to the inside of the electrolyte layer, thereby eliminating the need to form a multilayer electrolyte structure requiring a complicated manufacturing process as in the prior art. It is possible to manufacture a solid oxide fuel cell that can ensure durability against reverse voltage and also prevent leakage current.
  • cerium ions are diffused into an electrolyte layer composed of a single layer through a sintering process, thereby providing a locally electronic conductivity inside the electrolyte layer, as in the prior art. It is possible to manufacture a solid oxide fuel cell capable of securing durability against reverse voltage and preventing leakage current without forming a multilayer electrolyte structure requiring a complicated manufacturing process.

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

La présente invention concerne un procédé de fabrication d'une pile à combustible à oxyde solide dans laquelle une dégradation due à une tension de cellule négative est empêchée, le procédé comprenant : une étape de préparation d'une cellule unitaire de pile à combustible à oxyde solide dans laquelle une couche d'anode présentant une couche contenant de l'oxyde de cérium (CeO2) formée sur une surface de celle-ci, une couche d'électrolyte formée sur la couche contenant de l'oxyde de cérium et contenant de la zircone stabilisée par de l'oxyde d'yttrium (YSZ) et une couche de cathode sont empilées séquentiellement ; et (b) une étape de frittage de la cellule unitaire de pile à combustible à oxyde solide. Selon le procédé de fabrication d'une pile à combustible à oxyde solide (SOFC) de la présente invention, une pile à combustible à oxyde solide présentant une structure d'anode/électrolyte à gradient dans laquelle la concentration de cérium diminue progressivement de l'interface de couche d'anode/électrolyte au centre de la couche d'électrolyte peut être produite par le biais de l'étape de frittage dans laquelle des ions cérium diffusent dans la couche d'électrolyte à partir de la couche contenant de l'oxyde de cérium disposée dans l'anode. La pile à combustible à oxyde solide présente une conductivité du type N localement uniquement dans une section d'électrolyte à proximité de l'interface anode/électrolyte et peut ainsi empêcher efficacement une séparation anode/électrolyte dans des situations de tension de cellule négative. En outre, étant donné qu'une partie seulement de l'intérieur de l'électrolyte présente une conductivité du type N, des courants de fuite peuvent également être empêchés.
PCT/KR2019/008198 2018-07-17 2019-07-04 Procédé de fabrication d'une pile à combustible à oxyde solide permettant d'empêcher une dégradation sous une tension de cellule négative WO2020017796A1 (fr)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113097512A (zh) * 2021-03-31 2021-07-09 深圳大学 一种质子导体燃料电池及其制备方法

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EP0902493A1 (fr) * 1997-09-11 1999-03-17 Sulzer Hexis AG Elément électrochimique actif pour une pile à combustible à oxydes solides
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JPH08213028A (ja) * 1995-02-06 1996-08-20 Fujikura Ltd 固体電解質型燃料電池の燃料電極とその成膜方法
EP0902493A1 (fr) * 1997-09-11 1999-03-17 Sulzer Hexis AG Elément électrochimique actif pour une pile à combustible à oxydes solides
KR100648144B1 (ko) * 2005-09-15 2006-11-24 한국과학기술연구원 고성능 연료극지지형 고체산화물 연료전지
KR20120010507A (ko) * 2010-07-26 2012-02-03 삼성전기주식회사 고체 산화물 연료 전지 및 그 제조방법
KR20130047534A (ko) * 2011-10-28 2013-05-08 한국전력공사 Ｎｉ-ＹＳＺ 연료(수소)전극을 포함하는 고체산화물 연료전지와 전해셀 및 이의 제조방법

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CN113097512A (zh) * 2021-03-31 2021-07-09 深圳大学 一种质子导体燃料电池及其制备方法

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