WO2022153752A1 - 固体酸化物形燃料電池用ステンレス鋼材及びその製造方法、並びに固体酸化物形燃料電池用部材及び固体酸化物形燃料電池 - Google Patents

固体酸化物形燃料電池用ステンレス鋼材及びその製造方法、並びに固体酸化物形燃料電池用部材及び固体酸化物形燃料電池 Download PDF

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WO2022153752A1
WO2022153752A1 PCT/JP2021/045689 JP2021045689W WO2022153752A1 WO 2022153752 A1 WO2022153752 A1 WO 2022153752A1 JP 2021045689 W JP2021045689 W JP 2021045689W WO 2022153752 A1 WO2022153752 A1 WO 2022153752A1
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less
stainless steel
solid oxide
oxide fuel
steel material
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PCT/JP2021/045689
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English (en)
French (fr)
Japanese (ja)
Inventor
正治 秦野
三月 松本
善一 田井
一幸 景岡
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Nippon Steel Stainless Steel Corp
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Nippon Steel Stainless Steel Corp
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Priority to JP2022575144A priority Critical patent/JP7434611B2/ja
Priority to KR1020237010938A priority patent/KR20230060520A/ko
Priority to EP21919641.7A priority patent/EP4279624A4/en
Priority to CN202180071489.XA priority patent/CN116490632B/zh
Publication of WO2022153752A1 publication Critical patent/WO2022153752A1/ja
Anticipated expiration legal-status Critical
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • H01M8/0208—Alloys
    • H01M8/021—Alloys based on iron
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
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    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • 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

Definitions

  • the present invention relates to a stainless steel material for a solid oxide fuel cell and a method for producing the same, and a member for a solid oxide fuel cell and a solid oxide fuel cell.
  • the conventional solid oxide fuel cell is a high-temperature operating type with an operating temperature exceeding 600 ° C.
  • low-temperature operating solid oxide fuel cells that operate in a temperature range of 600 ° C. or lower have been proposed (for example, Patent Documents 1 and 2).
  • Stainless steel is generally used as a component of such a solid oxide fuel cell from the viewpoint of cost and corrosion resistance.
  • solid oxide fuel cells were mainly being developed as stationary power sources.
  • mobile vehicles such as commercial / industrial vehicles, automobiles, and airplanes.
  • the members for example, separators, interconnectors, current collectors, etc.
  • the members are required to have conductivity.
  • the conductivity of this member decreases as the operating temperature decreases, the member used in the conventional high-temperature operating type solid oxide fuel cell may not have sufficient conductivity.
  • it is required to make the member thinner and lighter. However, if the member is made thinner and lighter, thermal deformation is likely to occur.
  • the present invention has been made to solve the above problems, and is a stainless steel material for solid oxide fuel cells which has excellent conductivity at a temperature of 600 ° C. or lower and can suppress thermal deformation. It is an object of the present invention to provide the manufacturing method. Another object of the present invention is to provide a member for a solid oxide fuel cell and a solid oxide fuel cell provided with a stainless steel material for a solid oxide fuel cell having such characteristics.
  • the present inventors have found that the above problems can be solved by controlling the composition to a specific composition, and have completed the present invention. That is, in the present invention, C: 0.030% or less, Si: 1.00% or less, Mn: 1.00% or less, P: 0.050% or less, S: 0.0030% or less, based on mass.
  • the present invention is a member for a solid oxide fuel cell including the stainless steel material for the solid oxide fuel cell. Further, the present invention is a solid oxide fuel cell including the member for the solid oxide fuel cell.
  • a stainless steel material for a solid oxide fuel cell which has excellent conductivity at a temperature of 600 ° C. or lower and can suppress thermal deformation, and a method for producing the same. Further, according to the present invention, it is possible to provide a member for a solid oxide fuel cell and a solid oxide fuel cell provided with a stainless steel material for a solid oxide fuel cell having such characteristics.
  • the stainless steel material for solid oxide fuel cell (hereinafter abbreviated as "stainless steel material") according to the embodiment of the present invention has C: 0.030% or less, Si: 1.00% or less, Mn: 1.00%.
  • P 0.050% or less
  • S 0.0030% or less
  • Cr 22.0 to 32.0%
  • Mo 2.50% or less
  • N 0.030% or less
  • Al 0.30 % Or less
  • Nb 0.40% or less
  • Cu 1.00% or less
  • the effective Cr amount represented by the following formula (1) is It is 24.0 to 35.0% and has a composition in which the balance is composed of Fe and impurities.
  • the "impurity” is a component (for example, an unavoidable impurity) mixed with raw materials such as ore and scrap, and various factors in the manufacturing process when the stainless steel material is industrially manufactured, and is defined in the present invention. It means something that is acceptable as long as it does not adversely affect it.
  • the "stainless steel material” is a concept including various shapes such as a stainless steel strip, a stainless steel plate, and a stainless steel foil.
  • the stainless steel material according to the embodiment of the present invention has B: 0.0050% or less, Sn: 0.5% or less, V: 0.5% or less, W: 0.5% or less, if necessary.
  • C is an element that affects the conductivity of stainless steel materials at a temperature of 600 ° C. or lower. If the C content is too high, the conductivity will decrease. Therefore, the C content is 0.030% or less, preferably 0.020% or less, and more preferably 0.015% or less.
  • the lower limit of the C content is not particularly limited, but as the C content is reduced, the refining process takes more time, which may increase the manufacturing cost. Therefore, the C content is preferably 0.0002% or more, more preferably 0.0005% or more.
  • Si is an element effective for enhancing the heat resistance of stainless steel materials and obtaining the effect of forming a Cr oxide film and suppressing thermal deformation at 600 ° C. or lower.
  • the Si content is 1.00% or less, preferably 0.80% or less, more preferably 0.60% or less, still more preferably 0.30% or less.
  • the lower limit of the Si content is not particularly limited.
  • the Si content is preferably 0.05% or more, more preferably 0.08% or more, from the viewpoint of obtaining the above effects of Si.
  • Mn is an element effective for improving the conductivity of the oxide film by forming ( Mn, Cr) 3O4 type oxide as well as the toughness of the stainless steel material.
  • Mn content is 1.00% or less, preferably 0.50% or less.
  • the lower limit of the Mn content is not particularly limited.
  • the Mn content is preferably 0.05% or more, more preferably 0.08% or more, from the viewpoint of obtaining the above-mentioned effect of Mn.
  • P is an element that may reduce the toughness of the stainless steel material. Therefore, the P content is set to 0.050% or less, preferably 0.040% or less.
  • the lower limit of the P content is not particularly limited, but as the P content is reduced, the refining process takes more time, which may increase the manufacturing cost. Therefore, the P content is preferably 0.001% or more, more preferably 0.010% or more.
  • S is an element that produces sulfide-based inclusions and may reduce the power generation efficiency of SOFC due to evaporation and poisoning to the electrodes. Therefore, the S content is 0.0030% or less, preferably 0.0015% or less.
  • the lower limit of the S content is not particularly limited, but as the S content is reduced, the refining process takes more time, which may increase the manufacturing cost. Therefore, the S content is preferably 0.0001% or more, more preferably 0.0002% or more.
  • Cr is a main element for forming a passivation film on the surface of a stainless steel material, and the passivation film can improve properties such as corrosion resistance and heat resistance.
  • the Cr content is set to 22.0% or more, preferably 22.5% or more, from the viewpoint of forming a Cr oxide film having excellent conductivity at a temperature of 600 ° C. or lower and obtaining an effect of suppressing thermal deformation.
  • the Cr content is 32.0% or less, preferably 31.0% or less.
  • Mo is a main element for strengthening the passivation film of a stainless steel material, and the passivation film can improve properties such as corrosion resistance and heat resistance.
  • Mo is also an element that promotes the formation of a Cr oxide film of a stainless steel material at a temperature of 600 ° C. or lower to improve conductivity and lowers the coefficient of thermal expansion to suppress thermal deformation. Normally, since the Cr oxide generated at 600 ° C. or lower contains Fe, the conductivity is low, but the conductivity can be improved by allowing Mo in the Cr oxide. However, if the Mo content is too high, the toughness and the effect of suppressing thermal deformation may be impaired due to hardening.
  • the Mo content is 2.50% or less, preferably 2.00% or less, and more preferably 1.50% or less.
  • the lower limit of the Mo content is not particularly limited.
  • the Mo content is preferably 0.05% or more, more preferably 0.30% or more, from the viewpoint of obtaining the above-mentioned effect of Mo.
  • N is an element that binds to Al to generate AlN, which is the starting point of abnormal oxidation, and may reduce the toughness of the stainless steel material. Therefore, the N content is 0.030% or less, preferably 0.025% or less.
  • the lower limit of the N content is not particularly limited, but as the N content is reduced, the refining process takes more time, which may increase the manufacturing cost. Therefore, the N content is preferably 0.001% or more, more preferably 0.010% or more.
  • Al is an element effective for promoting the formation of a Cr oxide film at a temperature of 600 ° C. or lower of a stainless steel material and improving the conductivity.
  • the Al content is 0.30% or less, preferably 0.25% or less.
  • the lower limit of the Al content is not particularly limited.
  • the Al content is preferably 0.01% or more, more preferably 0.03% or more, from the viewpoint of obtaining the above effects of Al.
  • Nb is an element that preferentially combines with C and N to form Nb carbonitride, and thus increases the effective Cr amount of the stainless steel material. Therefore, Nb promotes the formation of a Cr oxide film at a temperature of 600 ° C. or lower and contributes to the improvement of conductivity. However, if the Nb content is too high, the amount of solid solution Nb that was not consumed in the formation of Nb carbonitride increases. As a result, the toughness and the effect of suppressing thermal deformation may be impaired due to the hardening. Therefore, the Nb content is 0.40% or less, preferably 0.35% or less. On the other hand, the lower limit of the Nb content is not particularly limited. The Nb content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the above-mentioned effect of Nb.
  • Ti is an element that increases the effective Cr amount of the stainless steel material because it preferentially bonds with C and N to form Ti carbonitride. Therefore, Ti promotes the formation of a Cr oxide film at a temperature of 600 ° C. or lower and contributes to the improvement of conductivity. However, if the Ti content is too high, the Ti carbonitride becomes coarse, which serves as a starting point and reduces the toughness and the effect of suppressing thermal deformation. Therefore, the Ti content is 0.40% or less, preferably 0.35% or less. On the other hand, the lower limit of the Ti content is not particularly limited. The Ti content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the above-mentioned effect of Ti.
  • the total content of Nb and Ti is not particularly limited, but is preferably 0.32% or more, more preferably 0.35% or more.
  • the ratio of the Nb content to the Ti content is not particularly limited, but is preferably 1.0 or less, more preferably 0.9 or less.
  • Ni is an element that suppresses the improvement of corrosion resistance and the decrease of toughness of stainless steel materials.
  • Ni is an austenite phase stabilizing element, if the Ni content is too large, the coefficient of thermal expansion increases and the effect of suppressing thermal deformation decreases. Therefore, the Ni content is 1.00% or less, preferably 0.80% or less.
  • the lower limit of the Ni content is not particularly limited. The Ni content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the above effects of Ni.
  • Cu is an element that improves the corrosion resistance and conductivity of stainless steel materials.
  • Cu is an austenite phase stabilizing element, if the Cu content is too large, the coefficient of thermal expansion increases and the effect of suppressing thermal deformation decreases. Therefore, the Cu content is 1.00% or less, preferably 0.80% or less.
  • the lower limit of the Cu content is not particularly limited. The Cu content is preferably 0.01% or more, more preferably 0.03% or more, from the viewpoint of obtaining the above effects of Cu.
  • Effective Cr amount 24.0 to 35.0%>
  • the effective Cr amount is represented by the following formula (1).
  • Effective Cr amount (%) Cr + 2Mo + 2Si + 5Nb + 2Ti-3 (2C + 3N + Ni + 0.5Mn + 0.2Cu) ...
  • each element symbol represents the content of each element.
  • Cr + 2Mo + 2Si + 5Nb + 2Ti represents a Cr equivalent
  • 2C + 3N + Ni + 0.5Mn + 0.2Cu represents a Ni equivalent.
  • the effective Cr amount is set to 35.0% or less, preferably 32.0% or less.
  • the effective Cr amount is 24.0% or more, preferably 25.0% or more.
  • B is an element effective for increasing the grain boundary strength and improving the secondary workability by preferentially concentrating the grain boundaries, and is contained in the stainless steel material as needed.
  • the B content is 0.0050% or less, preferably 0.0030% or less.
  • the lower limit of the B content is not particularly limited.
  • the B content is preferably 0.0002% or more, more preferably 0.0005% or more, from the viewpoint of obtaining the effect of B.
  • Sn is an element effective for improving corrosion resistance and conductivity, and is contained in a stainless steel material as needed. However, if the Sn content is too high, the hot workability and toughness deteriorate. Therefore, the Sn content is 0.5% or less, preferably 0.3% or less. On the other hand, the lower limit of the Sn content is not particularly limited. The Sn content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the effect of Sn.
  • V is an element that improves the strength of the stainless steel material without impairing the toughness of the stainless steel material, and is contained in the stainless steel material as needed.
  • the V content is 0.5% or less, preferably 0.4% or less.
  • the lower limit of the V content is not particularly limited.
  • the V content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the effect of V.
  • W is an element that improves the strength of the stainless steel material without impairing the toughness of the stainless steel material, and is contained in the stainless steel material as needed.
  • the W content is 0.5% or less, preferably 0.4% or less.
  • the lower limit of the W content is not particularly limited.
  • the W content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the effect of W.
  • Ca is an element that fixes S, enhances oxidation resistance, and promotes the formation of a Cr oxide film, and is contained in stainless steel materials as needed.
  • the Ca content is 0.0100% or less, preferably 0.0050% or less.
  • the lower limit of the Ca content is not particularly limited.
  • the Ca content is preferably 0.0005% or more, more preferably 0.0010% or more, from the viewpoint of obtaining the effect of Ca.
  • Mg is an element effective for refining stainless steel materials, and is contained in stainless steel materials as needed. However, if the Mg content is too high, the amount of inclusions produced increases and the effect of suppressing conductivity and thermal deformation is reduced. Therefore, the Mg content is 0.010% or less, preferably 0.005% or less. On the other hand, the lower limit of the Mg content is not particularly limited. The Mg content is preferably 0.0001% or more, more preferably 0.0005% or more, from the viewpoint of obtaining the effect of Mg.
  • Zr is an element that fixes C and increases the effective Cr amount of the stainless steel material, and is contained in the stainless steel material as needed. However, if the Zr content is too high, the workability of the stainless steel material will deteriorate. Therefore, the Zr content is 0.50% or less, preferably 0.40% or less. On the other hand, the lower limit of the Zr content is not particularly limited. The Zr content is preferably 0.001% or more, more preferably 0.005% or more, from the viewpoint of obtaining the effect of Zr.
  • Co is an element that improves the strength of the stainless steel material without impairing the toughness, and is contained in the stainless steel material as needed. However, if the Co content is too high, the workability and toughness may decrease, and the cost increases. Therefore, the Co content is 0.5% or less, preferably 0.4% or less. On the other hand, the lower limit of the Co content is not particularly limited. The Co content is preferably 0.01% or more, more preferably 0.05% or more, from the viewpoint of obtaining the effect of Co.
  • Ga is an element that improves the hot workability of the stainless steel material, and is contained in the stainless steel material as needed. However, if the Ga content is too high, the manufacturability will be reduced. Therefore, the Ga content is 0.01% or less, preferably 0.005% or less. On the other hand, the lower limit of the Ga content is not particularly limited. The Ga content is preferably 0.0001% or more, more preferably 0.0005% or more, from the viewpoint of obtaining the effect of Ga.
  • Hf is an element that fixes C and increases the effective Cr amount of the stainless steel material, and is contained in the stainless steel material as needed. However, if the Hf content is too high, the workability of the stainless steel material will deteriorate. Therefore, the Hf content is 0.10% or less, preferably 0.08% or less. On the other hand, the lower limit of the Hf content is not particularly limited. The Hf content is preferably 0.001%, more preferably 0.005%, from the viewpoint of obtaining the effect of Hf.
  • REM rare earth element
  • REM preferentially binds to S and P to form a compound, it is possible to suppress a decrease in conductivity and thermal deformation suppressing effect due to S and P.
  • REM is included in the stainless steel material as needed. However, if the REM content is too high, the stainless steel material may become hard and the toughness and workability may decrease. Therefore, the REM content is 0.10% or less, preferably 0.08% or less.
  • the lower limit of the REM content is not particularly limited.
  • the REM content is preferably 0.001% or more, more preferably 0.005% or more, from the viewpoint of obtaining the effect of REM.
  • REM is a general term for two elements, scandium (Sc) and yttrium (Y), and 15 elements (lanthanoids) from lanthanum (La) to lutetium (Lu). These may be used alone or as a mixture. Further, among REMs, La and Y are preferable.
  • the crystal orientation ratio ( ⁇ 211 ⁇ / ⁇ 200 ⁇ ) of the crystal orientation ⁇ 211 ⁇ to the crystal orientation ⁇ 200 ⁇ exceeds 1.5 at a depth of 10 ⁇ m from the surface. It is preferably less than 3.5, more preferably 2.0 to 3.0.
  • the conductivity of the stainless steel material at a temperature of 600 ° C. or lower mainly depends on the Cr concentration of the Cr oxide film ((Cr, Fe) 2 O 3 ) on the surface layer of the stainless steel material.
  • the crystal orientation ratio ( ⁇ 211 ⁇ / ⁇ 200 ⁇ ) within the above range, the orientation between the base metal and the Cr oxide film is improved, and the surface layer ((Cr, Fe) 2 O 3 ) Cr Since the concentration can be increased, the conductivity at a temperature of 600 ° C. or lower can be improved.
  • the crystal orientation is determined by X-ray diffraction on the surface of the stainless steel material. Specifically, a stainless steel material is cut, and the crystal orientation is measured on the surface thereof using an X-ray diffractometer (RINT 2500 manufactured by Rigaku Co., Ltd.).
  • ⁇ 200 ⁇ is detected at 65.20 ° and ⁇ 211 ⁇ is detected at 82.58 °, so the X-ray intensity ratio of those crystal planes is calculated.
  • the stainless steel material according to the embodiment of the present invention has a crystal orientation ⁇ 211 ⁇ with respect to a crystal orientation ⁇ 200 ⁇ at a position at the center in the thickness direction (position of t / 2 when the thickness of the stainless steel material is t).
  • the crystal orientation ratio ( ⁇ 211 ⁇ / ⁇ 200 ⁇ ) is preferably more than 0.5 and less than 2.0, and more preferably 0.5 to 1.5.
  • the thermal deformation of stainless steel is affected by the coefficient of linear expansion and Young's modulus at the position of the center in the thickness direction. Therefore, by controlling the crystal orientation ratio within the above range, the coefficient of linear expansion and Young's modulus decrease, so that thermal deformation can be suppressed.
  • the crystal orientation is determined by polishing (thinning) from the surface of the stainless steel material to t / 2 and X-ray diffraction on the surface. X-ray diffraction can be performed in the same manner as described above.
  • the shape of the stainless steel material according to the embodiment of the present invention is not particularly limited, but is preferably plate-shaped or foil-shaped.
  • its thickness is, for example, 0.1 to 5.0 mm, preferably 0.1 to 3.0 mm, more preferably 0.1 to 1.0 mm, still more preferably. Is 0.1 to 0.5 mm.
  • the stainless steel material according to the embodiment of the present invention can be produced according to a known method except that a slab having the above composition is used.
  • a slab having the above composition is used.
  • an example of a typical manufacturing method of the stainless steel material according to the embodiment of the present invention will be described.
  • the method for producing a stainless steel material according to the embodiment of the present invention is not limited to the following production method.
  • the stainless steel material according to the embodiment of the present invention can be produced by hot rolling a slab having the above composition and then cold rolling.
  • the conditions for hot rolling and cold rolling are not particularly limited and may be appropriately adjusted according to the composition. Before cold rolling, it is preferable that the hot-rolled material obtained by hot rolling is pickled and then surface-ground. Further, it is preferable that the hot-rolled material is pickled without annealing. Under such conditions, it becomes easy to control the crystal orientation of the stainless steel material within the above range.
  • the method of surface grinding is not particularly limited, and for example, a coil grinder can be used. At this time, the grinder count may be # 120 to 600 or the like.
  • the thickness of the surface grinding is not particularly limited, but is 0.005 to 0.100 mm. After cold rolling, known steps such as annealing and pickling may be carried out.
  • a passivation film is formed on the surface in an oxygen-containing atmosphere (for example, an atmospheric atmosphere).
  • This passivation film has excellent conductivity at a temperature of 600 ° C. or lower.
  • this stainless steel material is unlikely to undergo thermal deformation, it is suitable for solid oxide fuel cells, especially low-temperature operating solid oxide fuel cells that operate in a temperature range of 600 ° C. or lower (for example, 500 to 600 ° C.). Suitable for use.
  • the stainless steel material according to the embodiment of the present invention is used for a solid oxide fuel cell, a separator, a current collector (for example, an air electrode current collector and a fuel electrode current collector), an interconnector, a bus bar, and an end plate.
  • a stainless steel material can be used for members such as a fuel electrode frame.
  • the stainless steel material according to the embodiment of the present invention is preferably used for one or more kinds of members selected from a separator, an interconnector, and a current collector.
  • the solid oxide fuel cell member according to the embodiment of the present invention includes the stainless steel material according to the embodiment of the present invention. Further, the solid oxide fuel cell according to the embodiment of the present invention includes a member for the solid oxide fuel cell according to the embodiment of the present invention.
  • the member for a solid oxide fuel cell is not particularly limited, and examples thereof include the above-mentioned various members.
  • the stainless steel material can be appropriately shaped according to the shapes of various members.
  • a conductive coating layer may be formed on the surface of the stainless steel material.
  • the conductive coating layer is not particularly limited and can be formed from a material known in the art. For example, the conductive coating layer can be formed by using a metal having excellent conductivity such as Ag and Co.
  • the conductive coating layer may be a single metal layer or an alloy layer, and may have a single layer structure or a laminated structure.
  • the stainless steel material may be modified (roughened) of the passive film from the viewpoint of enhancing the adhesion to the conductive coating layer.
  • the passivation film can be modified (roughened) by a known method such as immersing a stainless steel material in a fluorinated nitric acid solution.
  • a slab having the composition shown in Table 1 is melted and hot-rolled to obtain a hot-rolled plate having a thickness of 3.5 mm, pickled without annealing, and 0.05 mm by a coil grinder (count 120). The surface was ground. Next, the surface-ground hot-rolled plate was cold-rolled to obtain a cold-rolled plate having a thickness of 0.1 to 0.6 mm, and then annealed and pickled to obtain a stainless steel material.
  • the products manufactured by this method are represented as "none" for hot-rolled sheet annealing and "yes” for surface grinding. Further, stainless steel was manufactured under the same conditions except that surface grinding was not performed in the above manufacturing method.
  • the products manufactured by this method are represented as “none” for hot-rolled sheet annealing and “none” for surface grinding. Further, a stainless steel material was also produced, which was hot-rolled under the same conditions as described above to obtain a hot-rolled plate, then annealed at 950 to 1050 ° C., pickled, and surface-ground and cold-rolled. In Table 2, the products manufactured by this method are represented by "yes” for hot-rolled sheet annealing and "yes” for surface grinding.
  • the evaluation method is as follows. (1) Surface modification is performed by immersing a conductive stainless steel material in an aqueous solution (liquid temperature 60 ° C.) containing 5.0% by mass of phosphoric acid and 15% by mass of nitric acid for 1 to 5 minutes, and then a coating treatment is performed. Was carried out to form a conductive coating layer. In the coating treatment, the surface of the surface-modified stainless steel material was adjusted so that Co-plating was formed with a thickness of 2 to 5 ⁇ m. Two stainless steel materials (hereinafter referred to as "stainless steel materials with a conductive coating layer") on which a conductive coating layer is formed are placed at 600 ° C.
  • a test piece for measurement as shown in FIG. 1 was prepared using these two stainless steel materials with a conductive coating layer, and measurement was performed by a four-terminal method using a potentiostat. Specifically, it was carried out as follows. First, a conductive paste (Ag paste) was applied in a square shape (10 mm on a side and 10 ⁇ m in thickness) to the central portion of the two stainless steel materials 10 with a conductive coating layer and dried to form the conductive portion 20.
  • a conductive paste Ag paste
  • the conductive portions 20 of the two stainless steel materials 10 with a conductive coating layer were stacked and arranged in a cross shape, sandwiched between alumina plates, placed with a weight (200 g), and baked in the electric furnace. (850 ° C. x 30 minutes).
  • the surface was scraped using a minitor until the metal base material was exposed to form the wiring attachment portion 30 shown in FIG.
  • a silver wire 40 ( ⁇ 0.3 mm) was wound around the wiring attachment portion 30, a conductive paste was applied, and the mixture was dried at 150 ° C. for 30 minutes to obtain a test piece for measurement.
  • this test piece for measurement was placed in a high-temperature electrochemical measuring device, and a voltage-current curve was obtained by a four-terminal method using a potentiostat.
  • the measurement temperature was 600 ° C. and the voltage was swept up to 10 mV.
  • the resistance value was calculated from the slope of the voltage-current curve.
  • A high temperature conductivity is particularly excellent
  • B high temperature conductivity
  • the case where the resistance value exceeds 30 m ⁇ ⁇ cm 2 is judged to be C (insufficient high temperature conductivity).
  • the thermal deformation of the stainless steel material was evaluated by the high temperature bending strength test method specified in JIS R1604: 2008. Specifically, a three-point bending method with a distance between external fulcrums of 30 mm was used, and a stainless steel material was cut to prepare a test piece of 4 mm ⁇ 40 mm. Next, the test piece and the three-point bending tester were housed in a muffle furnace, heated to 650 ° C. in the air, and then the bending strength at which the test piece was thermally deformed was measured.
  • test No. Since the stainless steel materials 1 to 14 (examples of the present invention) have a predetermined composition, they are excellent in conductivity and have a high effect of suppressing thermal deformation. In particular, Test No. Since the stainless steel materials 2, 7, 12 and 13 had a preferable composition and omitted the annealing of the hot-rolled plate, the crystal orientation ratio had a particularly preferable range and the conductivity was very good. .. In addition, the test No. From the comparison of 2 and 3, it was confirmed that by performing surface grinding, the crystal orientation ratio at a depth of 10 ⁇ m from the surface was in a preferable range, and the conductivity tended to be improved. On the other hand, the test No.
  • composition or effective Cr amount of the stainless steel materials of 15 to 21 (Comparative Example) was out of the predetermined range, conductivity and thermal deformation were obtained even if the thermal rolling sheet annealing was omitted and the stainless steel material had an appropriate crystal orientation.
  • a stainless steel material for a solid oxide fuel cell which has excellent conductivity at a temperature of 600 ° C. or lower and can suppress thermal deformation, and a method for producing the same. be able to. Further, according to the present invention, it is possible to provide a member for a solid oxide fuel cell and a solid oxide fuel cell provided with a stainless steel material for a solid oxide fuel cell having such characteristics.

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PCT/JP2021/045689 2021-01-14 2021-12-10 固体酸化物形燃料電池用ステンレス鋼材及びその製造方法、並びに固体酸化物形燃料電池用部材及び固体酸化物形燃料電池 Ceased WO2022153752A1 (ja)

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EP21919641.7A EP4279624A4 (en) 2021-01-14 2021-12-10 STAINLESS STEEL MATERIAL FOR SOLID OXIDE FUEL CELL AND METHOD FOR PRODUCING SAME, ELEMENT FOR SOLID OXIDE FUEL CELL, AND SOLID OXIDE FUEL CELL
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