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US20060193743A1 - Austenitic stainless steel for hydrogen gas and method for its manufacture - Google Patents

Austenitic stainless steel for hydrogen gas and method for its manufacture Download PDF

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Publication number
US20060193743A1
US20060193743A1 US11/297,418 US29741805A US2006193743A1 US 20060193743 A1 US20060193743 A1 US 20060193743A1 US 29741805 A US29741805 A US 29741805A US 2006193743 A1 US2006193743 A1 US 2006193743A1
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working
stainless steel
austenitic stainless
set forth
chemical composition
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Abandoned
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US11/297,418
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English (en)
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Hiroyuki Semba
Masaaki Igarashi
Tomohiko Omura
Mitsuo Miyahara
Kazuhiko Ogawa
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Nippon Steel Corp
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Individual
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Assigned to SUMITOMO METAL INDUSTRIES, LTD. reassignment SUMITOMO METAL INDUSTRIES, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SEMBA, HIROYUKI, OMURA, TOMOHIKO, OGAWA, KAZUHIRO, IGARASHI, MASAAKI, MIYAHARA, MITSUO
Publication of US20060193743A1 publication Critical patent/US20060193743A1/en
Priority to US12/953,576 priority Critical patent/US8696835B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • 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
    • Y02E60/32—Hydrogen storage

Definitions

  • This invention relates to a stainless steel for use in a hydrogen gas environment which has excellent mechanical properties (strength and ductility) and corrosion resistance and to a method for its manufacture.
  • the present invention relates to equipment used in a hydrogen gas environment such as piping, gas cylinders, and valves for hydrogen gas made from such a stainless steel.
  • a stainless steel according to the present invention is particularly suitable as a steel for structural equipment which is exposed to a high pressure hydrogen gas environment in fuel cell automobiles and hydrogen gas stations, and particularly for piping, gas cylinders, and valves.
  • fuel cell automobiles obtain electric power using hydrogen and oxygen as fuels. They have attracted attention as the next generation of clean automobiles which do not discharge carbon dioxide (CO 2 ) or harmful substances such as nitrogen oxides (NO x ) or sulfur oxides (SO x ) as do conventional gasoline-powered or diesel-powered automobiles.
  • CO 2 carbon dioxide
  • NO x nitrogen oxides
  • SO x sulfur oxides
  • Conventional methods thereof include a method in which a hydrogen gas cylinder is directly mounted on a vehicle, a method in which methanol or gasoline is reformed to obtain hydrogen by a reformer mounted on a vehicle, and a method in which a hydrogen-storing alloy which can absorb hydrogen is mounted on a vehicle.
  • FIG. 2 is a graph showing the relationship between the elongation in the direction perpendicular to the direction of working in cold working and the degree of cold working (hereunder referred to as “the percent reduction in cross section”). It can be seen that elongation greatly decreases as the degree of cold working increases. In actual practice, elongation of at least about 30% is desirable, but when the degree of cold working is large, a decrease in elongation becomes a problem.
  • the object of the present invention is to provide an austenitic stainless steel which has excellent mechanical properties and corrosion resistance and which can be used in a hydrogen gas environment such as one containing high pressure hydrogen gas at 70 MPa or above and to provide a method for its manufacture.
  • the present inventors studied the causes of a degradation in mechanical properties accompanying working of various types of austenitic stainless steels in detail. As a result of detailed study of the effects of the chemical composition and the metallic structure (the microstructure) of a material on a deterioration in mechanical properties, including hydrogen embrittlement in a high pressure hydrogen gas environment such as at least 70 MPa, and on corrosion resistance, they obtained the following new knowledge.
  • FIG. 3 is a graph showing the relationship between the degree of cold working and hydrogen embrittlement in the direction of working and the direction perpendicular thereto. The above-described tendency is clear therefrom.
  • a texture structure is achieved as the degree of cold working increases.
  • a rolled texture structure is formed such that ⁇ 112 ⁇ is parallel to the rolling surface and ⁇ 11 ⁇ overscore (1) ⁇ > is parallel to the direction of working (rolling), or such that ⁇ 110 ⁇ is parallel to the rolling surface and ⁇ 001> is parallel to the direction of working.
  • a fiber texture structure is formed in which ⁇ 11 ⁇ overscore (1) ⁇ > or ⁇ 001> is parallel to the direction of working (elongation).
  • Formation of such a texture structure can be measured by measurement of the x-ray integrated intensity I(hkl) (h, k, and l are Miller indices) obtained by x-ray diffraction of the rolling surface.
  • the degree of formation of the above-described texture structure can be obtained by measurement of the x-ray integrated intensity I(111) or I(002) for a cross section perpendicular to the direction of working.
  • the susceptibility to hydrogen embrittlement in the direction of working increases as the degree of formation of the x-ray integrated intensity I(111) of a cross section perpendicular to the direction of working increases.
  • the degree of the formation thereof exceeds 5
  • the susceptibility to hydrogen embrittlement indicated by elongation (hydrogen)/elongation (air) becomes ⁇ 0.75.
  • susceptibility to hydrogen embrittlement in the direction of working can be decreased.
  • elongation (hydrogen) means the elongation in a tensile test in a hydrogen gas environment
  • elongation (air) means the elongation in a tensile test in air.
  • FIG. 4 is a graph showing the relationship between the x-ray integrated intensity I(111) of a cross section perpendicular to the direction of working and resistance to hydrogen embrittlement for the direction of working and the direction perpendicular thereto. From FIG. 4 , it can be seen that the resistance to hydrogen embrittlement in the direction of working has a strong correlation to the x-ray integrated intensity I(111).
  • susceptibility to hydrogen embrittlement in the direction perpendicular to the direction of working has a correlation to the x-ray integrated intensity I(111) of a cross section perpendicular to the direction of working, it has an extremely strong correlation to the x-ray integrated intensity I(220) and the x-ray integrated intensity I(111) of a cross section in the direction of working.
  • the ratio I(220)/I(111) exceeds 10
  • susceptibility to hydrogen embrittlement enormously increases (susceptibility to hydrogen embrittlement as expressed by elongation (hydrogen)/elongation (air) ⁇ 0.75).
  • the x-ray integrated intensity ratio I(220)/I(111) of a plane in the direction of working is made 10 or less, susceptibility to hydrogen embrittlement perpendicular to the direction of working can be decreased.
  • FIG. 5 is a graph showing the relationship between the x-ray integrated intensity ratio I(220)/I(111) of a cross section in the direction of working and resistance to hydrogen embrittlement for the direction of working and the direction perpendicular thereto. From FIG. 5 , it can be seen that hydrogen embrittlement in the direction perpendicular to the direction of working has a strong correlation to the x-ray integrated intensity ratio I(220)/I(111).
  • the x-ray integrated intensity I(111) of a cross section perpendicular to the direction of working can be suppressed to at most 5 times that of a random direction, and the x-ray integrated intensity ratio I(220)/I(111) of a cross section in the direction of working can be suppressed to at most 10.
  • the x-ray integrated intensity ratio I(220)/I(111) of a cross section in the direction of working can be suppressed to at most 10.
  • the direction of working does not mean “the direction of plastic working itself” but means “the direction of plastic deformation of the material being worked”.
  • the present invention is an austenitic stainless steel for hydrogen gas having a chemical composition comprising, in mass percent, C: at most 0.10%, Si: at most 1.0%, Mn: 0.01-30%, P: at most 0.040%, S: at most 0.01%, Cr: 15-30%, Ni: 5.0-30%, Al: at most 0.10%, N: 0.001-0.30%, and a remainder of Fe and impurities and having a structure such that the x-ray integrated intensity I(111) of a cross section perpendicular to the direction of working is at most 5 times that of a random direction and such that the x-ray integrated intensity ratio I(220)/I(111) of a cross section in the direction of working is at most 10.
  • the direction of working herein means the direction of plastic deformation of the material being worked.
  • composition according to the present invention may further include at least one element selected from the following groups.
  • an austenitic stainless steel having the above-described chemical composition is subjected to plastic working with a reduction in cross section of 10-50% in a temperature range from room temperature to 200° C., and then plastic working of at least 5% is carried out in a direction different from the direction of working of the above-described plastic working.
  • FIG. 1 is a view showing the relationship between the degree of cold working and the tensile strength of a conventional steel.
  • FIG. 3 is a view showing that the resistance to hydrogen embrittlement in the direction of working greatly differs from that in the direction perpendicular to the direction of working.
  • FIG. 4 is a view showing that the resistance to hydrogen embrittlement in the direction of working has a strong correlation to the x-ray integrated intensity I(111) of a cross section in a direction perpendicular to the direction of working.
  • FIG. 5 is a view showing that the resistance to hydrogen embrittlement in the direction perpendicular to the direction of working has a strong correlation to the x-ray integrated intensity I(220)/I(111) of a cross section in the direction of working.
  • FIG. 6 is a view showing the relationship between grain diameter and resistance to hydrogen embrittlement in examples.
  • the content of C is made at most 0.10%.
  • M is Cr, Mo, Fe, or the like
  • MC-type carbides M is Ti, Nb, Ta, or the like
  • C is limited to at most 0.10%.
  • Nb greater than 0.20% and at most 1.0%
  • Ta greater than 0.40% and at most 1.0%
  • Ti greater than 0.10% and at most 1.0% in order to obtain a higher strength
  • C+N is limited to at most 0.05%.
  • Si is known as an element which is effective for improving corrosion resistance in various environments, but if a large amount thereof is added, it forms intermetallic compounds with Ni, Cr, and the like, it promotes the formation of sigma phase and other intermetallic compounds, and there are cases in which it markedly lowers hot workability. Therefore, the content of Si is made at most 1.0% and preferably at most 0.5%. In the same manner as for C, taking into consideration the refining costs of Si, it is not necessary to make the content of Si zero, and preferably it is at least 0.001%.
  • Mn is not only effective in minute amounts as a deoxidation and desulfurization agent, but in addition, there are cases in which it is added in large amounts as an inexpensive austenite stabilizing element.
  • Mn is added in an amount of at least 0.01%. However, if it exceeds 30%, there are cases in which hot workability and weathering resistance decrease, so it is made 0.01-30%. Preferably it is 0.1-20%.
  • Cr is essential as an element for improving corrosion resistance in the above-described environment of use, so it is included in an amount of at least 15%. However, if a large amount is added, a large amount of nitrides such as CrN and Cr 2 N or M 23 C 6 -type carbides are formed, so the content of Cr is made 15-30%. Preferably it is 15-27%.
  • Al is an important element as a deoxidizing agent. However, if a large amount remains in excess of 0.10%, it promotes the formation of sigma phase and other intermetallic compounds, which is undesirable from the standpoint of achieving the strength and toughness which are the objects of the present invention.
  • N is an important solid solution strengthening element. When it is included in a suitable range in conjunction with Mn, Cr, Ni, C, and the like, it suppresses the formation of sigma phase and other intermetallic compounds, and it contributes to an increase in toughness, particularly in the direction perpendicular to the direction of working. For this purpose at least 0.001% is added. However, if it is added in excess of 0.30%, cold workability decreases, so it is made 0.001-0.30%.
  • Nb greater than 0.20% and at most 1.0%
  • Ta greater than 0.40% and at most 1.0%
  • Ti greater than 0.10% and at most 1.0% with the object of obtaining a higher strength
  • C+N is restricted to a range of at most 0.05%.
  • V, Nb, Ta, Ti, Zr, and Hf form cubic carbonitrides and contribute to an increase in strength, and if necessary at least one of these may be added. However, if a large amount of carbonitrides thereof precipitate, ductility and toughness in the direction perpendicular to the direction of working decrease, and the contents thereof in the steel according to the present invention are each made 0.001-1.0%.
  • At least one of Nb, Ta, and Ti is contained in the ranges of Nb: greater than 0.20% and at most 1.0%, Ta: greater than 0.40% and at most 1.0%, and Ti: greater than 0.10% and at most 1.0%, and C+N is preferably restricted to the range of at most 0.05%.
  • B contributes to refinement of precipitates and refinement of austenite crystal grain, and if necessary at least 0.0001% of B may be added. However, if a large amount of B is added, it forms low melting point compounds, and there are cases in which it decreases hot workability. Thus, its upper limit is made 0.020%.
  • Cu and Co are austenite stabilizing elements.
  • they when they are suitably combined with Mn, Ni, C, or Cr, they contribute to an increase in strength, and optionally, at least one thereof may be added in an amount of at least 0.3%.
  • the content thereof is defined as Cu: 0.3-2.0% and Co: 0.3-5.0%.
  • Mg, Ca, and, of the transition elements, La, Ce, Y, Sm, Pr, and Nd act to prevent occurrence of cracks during solidification at the time of casting when present in the ranges set forth for the steel of the present invention, and they have the effect of reducing a decrease in ductility resulting from hydrogen embrittlement after long periods of use. If necessary, therefore, at least one of any of Mg: 0.0001-0.0050%, Ca: 0.0001-0.0050%, La: 0.0001-0.20%, Ce: 0.0001-0.20%, Y: 0.0001-0.40%, Sm: 0.0001-0.40%, Pr: 0.0001-0.40%, and Nd: 0.0001-0.50% may be added.
  • An austenitic stainless steel according to the present invention has a tensile strength on the level of at least 800 MPa and preferably at least 900 MPa, and it has an elongation of at least 30%.
  • the steel can be used in the form of plates, pipes, rods, shaped members, and wire, for example. If necessary, it can further undergo surface treatment such as plating.
  • the directions of working are preferably perpendicular to each other.
  • the direction of working refers to the direction of plastic deformation of the material being worked.
  • the direction of working is the lengthwise direction of the steel pipe, and when carrying out swaging to compress a steel pipe, it is the radial direction of the steel pipe.
  • the order in which the first and second cold working are performed is usually such that the working with the larger degree of working is carried out first and then the working with the smaller degree of working is carried out.
  • such a texture structure is obtained in order to improve resistance to hydrogen embrittlement, and it is sufficient to form such a texture structure at least in a surface layer portion where contact with a hydrogen gas atmosphere takes place. Accordingly, after pipe forming, it is permissible to eliminate anisotropy of the texture structure only in the surface layer portion (the inner surface or the outer surface of the pipe) by shot peening.
  • Table 1 shows examples of the chemical composition (mass percent) of an austenitic stainless steel according to the present invention and of a comparative steel.
  • Manufacturing Steel C Si Mn P S Cr Ni sol-Al N Mo W others process Present invention 1 0.005 0.39 1.78 0.018 0.0007 18.2 9.5 0.009 0.045 A 2 0.016 0.36 1.03 0.001 0.0008 25.6 20.7 0.011 0.089 B 3 0.018 0.40 2.36 0.027 0.0007 27.8 28.7 0.007 0.152 A 4 0.014 0.43 10.51 0.010 0.0008 18.9 10.3 0.006 0.281 A 5 0.015 0.47 15.23 0.019 0.0007 24.1 21.1 0.010 0.279 A 6 0.020 0.38 1.78 0.029 0.0008 16.4 12.7 0.009 0.090 2.14 B 7 0.046 0.46 9.12 0.004 0.0010 16.8 13.0 0.006 0.275 2.46 A 8 0.004 0.39 1.73 0.025 0.0008 16.5 12.2
  • the water-cooled plates were subjected to cold rolling of 30%, after which cold rolling of 10% was carried out in the direction perpendicular to the previous direction of working (manufacturing method A), or the water-cooled plates were subjected to cold rolling of 40% and then to cold rolling of 10% in the direction perpendicular to the previous direction of working (manufacturing method B) to obtain test materials.
  • test materials For comparative steels B-G, after the above-described hot forging and solid solution treatment, cold rolling of 10-65% in a single direction was carried out to obtain test materials.
  • test materials were obtained by the above-described manufacturing method B.
  • test materials For comparative steels N and O, after hot forging and solid solution treatment, cold rolling of 50% was carried out in a single direction to obtain test materials.
  • steels of the present invention of Nos. 1-32 of Table 2 each had an x-ray integrated intensity I(111) of a cross section in the direction perpendicular to the direction of working (a cross section perpendicular to the direction of working) of at most 5 times that in a random direction, and the x-ray integrated intensity ratio I(220)/I(111) of a cross section in the direction of working (a working direction cross section) of at most 10.
  • the strength TS at room temperature was at least 800 MPa
  • YS was at least 400 MPa
  • elongation was at least 30%.
  • susceptibility to hydrogen embrittlement which was evaluated by the ratio of the ductility in a tensile test in a hydrogen gas environment to that in a tensile test in air was extremely low.
  • cold rolling was carried out twice on a plate in different directions of working, but the same effects as in this example can be obtained when carrying out cold rolling two times in different directions of working on a steel pipe (such as pipe forming by cold drawing and pipe expansion with a plug).
  • an austenitic stainless steel which has excellent mechanical properties (strength and ductility) and corrosion resistance for use as a component of structural equipment which is exposed to high pressure hydrogen gas, specifically which is used in a hydrogen environment such as in a fuel cell automobile or a hydrogen gas station.

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US11/297,418 2003-06-10 2005-12-09 Austenitic stainless steel for hydrogen gas and method for its manufacture Abandoned US20060193743A1 (en)

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PCT/JP2004/008380 WO2004111285A1 (fr) 2003-06-10 2004-06-09 Acier inoxydable austénitique destiné à être utilisé en présence d'hydrogène et procédé de production dudit acier

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US20090159602A1 (en) * 2005-11-01 2009-06-25 Masaharu Hatano Austenitic High Mn Stainless Steel for High Pressure Hydrogen Gas
US20100034689A1 (en) * 2007-10-03 2010-02-11 Hiroyuki Hirata Austenitic stainless steel
US20100054983A1 (en) * 2007-10-04 2010-03-04 Takahiro Osuki Austenitic stainless steel
US20110024005A1 (en) * 2007-07-20 2011-02-03 Sumitomo Metal Industries, Ltd. Method for Producing Two-Phase Stainless Steel Pipe
US20120003116A1 (en) * 2009-03-27 2012-01-05 Sumitomo Metal Industries, Ltd. Austenitic stainless steel
US20130174949A1 (en) * 2010-09-29 2013-07-11 Nippon Steel & Sumikin Stainless Steel Corporation Austenitic high mn stainless steel and method production of same and member using that steel
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US11149324B2 (en) 2015-03-26 2021-10-19 Nippon Steel Stainless Steel Corporation High strength austenitic stainless steel having excellent resistance to hydrogen embrittlement, method for manufacturing the same, and hydrogen equipment used for high-pressure hydrogen gas and liquid hydrogen environment
US20220213571A1 (en) * 2019-05-31 2022-07-07 Nippon Steel Corporation Austenitic stainless steel material
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KR100666727B1 (ko) * 2005-04-19 2007-01-09 포스코신기술연구조합 스프링용 ３０４ｈ 오스테나이트계 스테인레스강
US20060275168A1 (en) * 2005-06-03 2006-12-07 Ati Properties, Inc. Austenitic stainless steel
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CN101135028B (zh) * 2006-08-30 2010-08-11 宝山钢铁股份有限公司 一种高强度不锈钢及其热处理方法
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EA200800023A1 (ru) * 2006-10-02 2008-06-30 Дмитрий Владимирович Савкин Жаропрочная коррозионно-стойкая сталь
KR100832487B1 (ko) * 2006-12-22 2008-05-26 한국항공우주연구원 초저온에서 높은 항복강도 및 우수한 연신율을 갖는 고강도스테인리스 스틸
EP2119802B1 (fr) 2007-01-15 2019-03-20 Nippon Steel & Sumitomo Metal Corporation Joint soudé d'acier inoxydable austénitique et matériau de soudage d'acier inoxydable austénitique
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