WO2022153731A1 - 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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Publication number
WO2022153731A1
WO2022153731A1 PCT/JP2021/045168 JP2021045168W WO2022153731A1 WO 2022153731 A1 WO2022153731 A1 WO 2022153731A1 JP 2021045168 W JP2021045168 W JP 2021045168W WO 2022153731 A1 WO2022153731 A1 WO 2022153731A1
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less
stainless steel
solid oxide
oxide fuel
steel material
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PCT/JP2021/045168
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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 JP2022575137A priority Critical patent/JP7825805B2/ja
Priority to EP21919620.1A priority patent/EP4279623A4/en
Priority to CN202180071487.0A priority patent/CN116490631B/zh
Priority to KR1020237010939A priority patent/KR20230060521A/ko
Publication of WO2022153731A1 publication Critical patent/WO2022153731A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
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    • 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
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    • C21D6/00—Heat treatment of ferrous alloys
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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
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
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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
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
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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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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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    • C—CHEMISTRY; METALLURGY
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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
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    • 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
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    • H01M8/10—Fuel cells with solid electrolytes
    • H—ELECTRICITY
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    • 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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    • C21—METALLURGY OF IRON
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    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
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    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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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.) constituting the solid oxide fuel cell 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.
  • the members used in the conventional stationary solid oxide fuel cell have sufficient thermal shock resistance.
  • the present invention has been made to solve the above problems, and provides a stainless steel material for a solid oxide fuel cell having excellent conductivity and thermal shock resistance at a temperature of 600 ° C. or lower, and a method for producing the same.
  • the purpose is to do.
  • 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 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.
  • the present invention it is possible to provide a stainless steel material for a solid oxide fuel cell having excellent conductivity and thermal shock resistance at a temperature of 600 ° C. or lower, 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 13.0% or more and less than 22.0%
  • Mo 1.50% or less
  • N 0.030% or less
  • Al 0.030% or less
  • Al Al: 0 .30% or less
  • Nb 0.40% or less
  • Cu 1.00% or less
  • the high purity index is less than 1.50%.
  • 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 that enhances the heat resistance of stainless steel materials and is effective in forming a Cr oxide film 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 13.0% or more, preferably 13.5% or more.
  • the Cr content is less than 22.0%, preferably 21.0% 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 at a temperature of 600 ° C. or lower for stainless steel materials to improve conductivity. 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 thermal impact resistance may decrease due to hardening. Therefore, the Mo content is 1.50% or less, preferably 1.30% or less, and more preferably 1.00% or less. On the other hand, 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 preferentially combines with C and N to form Nb carbonitride, and is therefore an effective element for purifying stainless steel materials. 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. Further, Nb is also an element that suppresses a decrease in corrosion resistance due to the formation of Cr carbonitride. 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 thermal impact resistance may decrease 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 preferentially combines with C and N to form Ti carbonitride, and is therefore an effective element for purifying stainless steel materials. 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. Ti is also an element that suppresses a decrease in corrosion resistance due to the formation of Cr carbonitride. However, if the Ti content is too high, the Ti carbonitride becomes coarse, which causes a decrease in toughness and thermal shock resistance. 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 effects of Ti.
  • 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 thermostable impact resistance 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 thermostable impact resistance 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.
  • High purity index 10 (C + N) + 15S + 8P + 2 (Ti + Nb) ... (1)
  • each element symbol represents the content of each element. If the high purity index is too high, the amount of Cr in the surface layer of the stainless steel material is consumed by the formation of carbonitride and the like, and the formation of the Cr oxide film at a temperature of 600 ° C. or lower is impaired. As a result, along with the decrease in conductivity, cracks are likely to occur in the surface layer starting from the carbonitride, which leads to a decrease in thermal impact resistance.
  • the high purity index is less than 1.50%, preferably 1.30% or less, and more preferably less than 1.00%.
  • the lower limit of the high purity index is not particularly limited.
  • the high purity index is preferably 0.30% or more, more preferably 0.40% or more, in order to suppress an excessive refining load and an increase in raw material cost.
  • 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 above-mentioned effect of B.
  • Sn is an element effective for improving the corrosion resistance and conductivity of the stainless steel material, and is contained in the 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 above-mentioned 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 above-mentioned 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 above-mentioned effect of W.
  • Ca is an element that fixes S and is effective for purifying the stainless steel material, and is contained in the stainless steel material as needed.
  • the Ca content is 0.010% or less, preferably 0.005% 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 above-mentioned 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 formed increases and the conductivity and thermal impact resistance are lowered. 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 above effects of Mg.
  • Zr is an element that fixes C and is effective for purifying 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 above-mentioned 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 above effects 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 above-mentioned effect of Ga.
  • Hf is an element that fixes C and is effective for purifying 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 above-mentioned effect by 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 impact resistance 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 above-mentioned effect by 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 stainless steel material according to the embodiment of the present invention has a crystal orientation ratio ( ⁇ 200 ⁇ / [ ⁇ 110) of crystal orientation ⁇ 200 ⁇ to a total of crystal orientations ⁇ 110 ⁇ and ⁇ 211 ⁇ at a depth of 10 ⁇ m from the surface.
  • ⁇ + ⁇ 211 ⁇ ] is preferably less than 0.30, and more preferably 0.25 or less.
  • the lower limit of the crystal orientation ratio is not particularly limited, but is preferably 0.05 or more, more preferably 0.10 or more.
  • the decrease in thermal shock resistance of the stainless steel material is due to the fact that cracks are likely to occur in the surface layer due to the difference between the texture of the surface layer of the stainless steel material and the texture of the matrix of the stainless steel material.
  • the surface layer of the stainless steel material has many crystal orientations ⁇ 200 ⁇ having a small plastic deformability, cracks are likely to occur. Therefore, by controlling the crystal orientation ratio ( ⁇ 200 ⁇ / [ ⁇ 110 ⁇ + ⁇ 211 ⁇ ]) to less than 0.30, the ratio of the crystal orientation ⁇ 200 ⁇ that is the starting point of the crack is reduced, and the crack is generated.
  • the heat impact resistance can be improved by suppressing the above.
  • the conductivity of the stainless steel material at a temperature of 600 ° C. or lower depends on the decrease in the Cr concentration of the Cr oxide film ((Cr, Fe) 2 O 3 ) formed on the surface layer of the stainless steel material.
  • the crystal orientation ratio ( ⁇ 200 ⁇ / [ ⁇ 110 ⁇ + ⁇ 211 ⁇ ]) to less than 0.30, the orientation with the Cr oxide film is improved and the surface layer ((Cr, Fe)). Since the Cr concentration of 2 O 3 ) can be increased, the conductivity at a temperature of 600 ° C. or lower can be improved.
  • the stainless steel material according to the embodiment of the present invention has a crystal orientation ⁇ 111 ⁇ ⁇ 15 ° ratio of 60 at the position of the central portion in the thickness direction (position of t / 2 when the thickness of the stainless steel material is t). It is preferably in excess of%, more preferably 65% to 99%. The upper limit of this ratio is preferably 98%, more preferably 95%.
  • the ratio of crystal orientation ⁇ 111 ⁇ ⁇ 15 ° can be measured by an EBSP orientation analysis system that can visualize the crystal orientation of each crystal grain. Specifically, a stainless steel material is cut, polished (thinned) from the surface to t / 2, and the surface is subjected to colloidal silica polishing to remove processing strain and EBSP orientation analysis is performed. For example, it is preferable to capture a region having a width of 1 mm and a length of 2 mm for the orientation analysis.
  • the ratio of ⁇ 111 ⁇ ⁇ 15 ° can be obtained by dividing the crystal orientation map display of the EBSP orientation analysis system into a region consisting of ⁇ 111 ⁇ ⁇ 15 ° and other orientations.
  • 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.
  • Cold rolling after hot rolling can include intermediate rolling and finish rolling.
  • the intermediate rolling is preferably performed using a large-diameter roll having a diameter of 100 mm or more. By performing intermediate rolling using such a large-diameter roll, strain can be easily introduced in the vicinity of the center of the plate thickness in addition to the surface layer, so that the crystal orientation can be easily controlled as described above.
  • Finish rolling is preferably performed using a small diameter roll.
  • cold rolling is generally carried out using a multi-stage small-diameter roll such as a Zendimia mill.
  • Cold rolling of large-diameter rolls can be performed, for example, by using a tandem mill rolling mill used for cold rolling of carbon steel.
  • the cold-rolled material obtained by cold rolling is preferably pickled and then surface-ground. Under such conditions, it becomes easy to control the crystal orientation of the stainless steel material within the above range.
  • the surface grinding method is not particularly limited, and for example, buffing, grindstone polishing, or the like can be used.
  • the thickness of the surface grinding is not particularly limited, but is 0.001 to 0.050 mm. After hot 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 also excellent in thermal shock resistance, it is a solid oxide fuel cell, particularly a low temperature operation type solid oxide fuel cell that operates in a temperature range of 600 ° C. or lower (for example, 500 to 600 ° C.). Suitable for use in fuel cells.
  • 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 passivation film from the viewpoint of enhancing the adhesion to the conductive coating layer.
  • the modification (roughening) of the passivation film can be performed by a known method such as immersing a stainless steel material in a fluorinated nitric acid solution.
  • the slab having the composition shown in Table 1 was melted, heated to 1200 ° C., and then hot-rolled to obtain a hot-rolled plate having a thickness of 3.0 mm.
  • the hot-rolled sheet was annealed and pickled, and then cold-rolled.
  • cold rolling a hot-rolled sheet is intermediate-rolled at 40-60% using a large-diameter roll having a diameter of 100 mm, then intermediate-annealed and pickled, and then finish-rolled on a small-diameter roll to 0.1- A 0.5 mm cold rolled plate was used.
  • the cold-rolled plate was finish-annealed and pickled, and the surface was ground by 0.005 to 0.01 mm by polishing with a grindstone to obtain a stainless steel material. Further, in the cold rolling, a stainless steel material obtained by cold rolling the intermediate rolling with the same small diameter roll as the finish rolling was also produced. Table 2 shows the roll diameters used in the intermediate rolling.
  • the crystal orientations ⁇ 110 ⁇ , ⁇ 211 ⁇ and ⁇ 200 ⁇ at a depth of 10 ⁇ m from the surface were measured, and the crystal orientation ratio ( ⁇ 200 ⁇ / [ ⁇ 110 ⁇ + ⁇ 211 ⁇ ])) was obtained. Moreover, the ratio of the crystal orientation ⁇ 111 ⁇ ⁇ 15 ° at the position of the central portion in the thickness direction was measured. The crystal orientation was measured under the above conditions. The results are shown in Table 2.
  • 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.
  • 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.
  • 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 measurement test piece was placed in a high-temperature electrochemical measuring device, and a voltage-current curve was obtained by a four-terminal method using a potentiostat. In this measurement, the measurement temperature was 600 ° C. and the voltage was swept up to 10 mV. Moreover, the resistance value was calculated from the slope of the voltage-current curve.
  • the heat-resistant impact resistance was evaluated by repeating the heating / cooling cycle of the above-mentioned stainless steel material with a conductive coating layer. Specifically, the above-mentioned stainless steel material with a Co-plated conductive coating layer was cut and processed to prepare a 10 mm ⁇ 25 mm test piece. Next, the test piece is housed in a mobile muffle furnace heated to 600 ° C., held in the atmosphere for 25 minutes (inside the muffle furnace), released to the atmosphere and cooled for 5 minutes (muffle furnace movement) as one cycle, and 100 cycles. An intermittent heating test was conducted.
  • test No. 16 is conductivity
  • test No. 18 to 20 had insufficient thermal impact resistance.
  • the present invention it is possible to provide a stainless steel material for a solid oxide fuel cell having excellent conductivity and thermal shock resistance at a temperature of 600 ° C. or lower, 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.

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PCT/JP2021/045168 2021-01-14 2021-12-08 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 WO2022153731A1 (ja)

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