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    • 专利摘要:
    HIGH AUSTENITIC STAINLESS STEELRESISTANCE TO HIGH PRESSURE HYDROGEN GAS It is austenitic stainless steel for high hydrogen gaspressure consisting, in percentage by mass, of C: 0.10% or less, Si: 1.0% or less, Mn: 3% or more to less than 7%, Cr: 15 to 30%, Ni: 10% ormore than less than 17%, AI: 0.10% or less, N: 0.10 to 0.50% and at leasta type of V: 0.01 to 1.0% and Nb: 0.01 to 0.50%, the balance being Fe andimpurities, where the impurities, the P content is 0.050% or less and the Pof S is 0.050% or less, the tensile strength is 800 MPa or more, the grain size number (ASTM E112) is No. 8 or more and carbonitrides of alloy that have a maximum diameter of 50 to 1,000 nm are contained in theamount of 0.4 < 109 > m ^ 2 ^ or more in the section observationtransversal.
    公开号:BR112013018100A2
    申请号:R112013018100-1
    申请日:2012-03-19
    公开日:2021-02-23
    发明作者:Tomohiko Omura；Jun Nakamura；Hirozaku Okada；Hiroyuki Semba；Yusaku Tomio；Hiroyuki Hirata；Masaaki Igarashi；Kazuhiro Ogawa；Masaaki Terunuma
    申请人:Nippon Steel & Sumitomo Metal Corporation；
    IPC主号:
    专利说明:

    “HIGH-RESISTANCE AUSTENITIC STAINLESS STEEL FOR HIGH PRESSURE HYDROGEN GAS” Field of the Technique The present invention relates to a high-strength stainless steel for high-pressure hydrogen gas, which has a tensile strength of 800 MPa or more and has excellent mechanical properties in a high pressure hydrogen gas environment.
    Prior Art In recent years, the development of racing fuel cell vehicles works with the use of hydrogen as the fuel and research on practical hydrogen stations to supply hydrogen to fuel cell vehicles has been advanced. Stainless steel is one of the candidate materials used for these applications; but, in a high pressure hydrogen gas environment, stainless steel may be susceptible to embrittlement caused by hydrogen gas (hydrogen embrittlement). In accordance with the Exemplified Compressed Hydrogen Vehicle Container Standards stipulated in the High Pressure Gas Safety Act, the use of austenitic SUS316L is approved as a stainless steel that is not susceptible to hydrogen embrittlement.
    In consideration of the need for reduced fuel cell vehicle weight and high pressure hydrogen station operation, however, for a stainless steel used for a container and a pipe, there has been a need for stainless steel that has a higher strength than that of the existing SUS316L, especially a tensile strength of 800 MPa or more and is not susceptible to embrittlement of the hydrogen environment in a hydrogen gas environment. That is, assuming the use of high pressure hydrogen of about 70 MPa, it is estimated that SUS316L requires a pipe and a container to have a wall thickness of 20 mm or more, which leads to a significant increase in the weight of vehicle empty, so that superior steel strength is indispensable.
    As a method of enhancing the strength of steel, cold rolling can be cited as a typical method.
    Patent Document 1 generates a description in relation to cold rolling and the hydrogen defragilizing property of austenitic stainless steel.
    As a means of strengthening austenitic stainless steel and enhancing the hydrogen embrittlement property of austenitic stainless steel without relying on cold rolling strength, Patent Documents 2 and 3 propose high strength stainless steels for high pressure hydrogen gas, where precipitation strengthening using fine nitrides is used.
    Patent Document 2 proposes a high strength austenitic stainless steel in which 7 to 30% Mn, 15 to 22% Cr, and 5 to 20% Ni are contained as the main components, and Patent Document 3 proposes stainless steel high strength austenitic in which 3 to 30% Mn, more than 22% to 30% or less Cr, and 17 to 20% Ni are contained as main components.
    These Documents indicate that a tensile strength of 800 MPa or more can be achieved in a state of heat treatment of solid solution.
    Citation List Patent Document Patent Document 1 WO 2004/111285 Patent Document 2 WO 2004/083477 Patent Document 3 WO 2004/083476 Summary of the Invention Technical Problem In Patent Document 1, the influence of cold rolling on embrittlement of hydrogen environment was also studied for SUS316L, in which it is verified that the cold lamination in the reduction of area of 30% or less does not have a great influence on the embrittlement property of hydrogen environment, which indicates the possibility that. a tensile strength of about 800 MPa can be achieved by cold rolling in an area reduction of 20 to 30%. However, high strength austenitic stainless steel has a problem of decreased elongation and weakening of the hydrogen environment by cold rolling.
    The invention described in Patent Document 1 reveals, as measures against this problem, a technique in which cold rolling is carried out in two or more stages, and when cold rolling is carried out in different rolling directions, the decrease in property weakening of the hydrogen environment and the decrease in elongation are contained; however, the application of this invention inevitably requires considerably complicated cold rolling.
    In addition, in the event that a cold-rolled material is welded, local softening may be caused by the effect of de-soldering heat.
    Therefore, it is difficult to join the materials by a welded joint, and the material joint is restricted to a mechanical joint.
    To reduce the weight of the fuel cell vehicle or to streamline the plumbing system for the hydrogen station, there was a strong need for stainless steel that has a high strength and is not a problem even if it is welded.
    In this case, such a means to achieve cold rolling strengthening is difficult to apply in some respects.
    The austenitic stainless steels described in Patent Documents 2 and 3 achieve a high strength of 800 MPa or more in a state after heat treatment of solid solution.
    However, in Patent Document 2, when the Mn content is less than 7%, a sufficient hydrogen embrittlement property cannot be obtained and sufficient strength cannot be achieved in a solid solution heat treatment state.
    In addition, in the steel related to Patent Document 3, both the Cr concentration and the Ni concentration are considerably high, so that this steel has a considerably high alloy cost disadvantage.
    The austenitic stainless steel described in Patent Document 2 can be produced at a somewhat low alloy cost compared to the steel described in Patent Document 3. Therefore, if stainless steel can be used in high pressure hydrogen applications even if stainless steel has a low Mn content of less than 7% compared to Patent Document 2, an advantage is brought about in industrial production, as steels in this range of Mn content have been used conventionally in applications such as the nuclear field and a common ingot can be used.
    The present invention was made in view of the present situation and therefore an objective of the same is to provide an austenitic stainless steel that has a high strength so that the tensile strength is 800 MPa or more and is excellent in the embrittlement property of hydrogen environment in the composition range of less than 7% Mn, whose austenitic stainless steel has not been materialized in the Patent Document
    2. Solution to the Problem The present inventors conducted several studies to solve the problem and reluctantly obtained the findings described in items (a) to (d) below.
    (a) Using nitrogen as a solute element, the strength of stainless steel can be enhanced. However, the addition of a large amount of nitrogen decreases the stacking failure energy and therefore has an adverse influence so that the distortion at the moment of deformation is located and the durability against hydrogen embrittlement is decreased.
    (b) By making fine grains, the resistance to embrittlement of high-nitrogen steel hydrogen environment can be enhanced.
    As a method for making the grains thin, there is a method in which precipitating fine alloy carbonitrides at the time of heat treatment of the final solid solution, the growth of the grains is restrained by the pinning effect.
    In order to produce fine carbonitrides and to make steel grains with high nitrogen content thin, it is more effective to add V or Nb.
    However, in the conventional method, although V and Nb precipitated as nitrides, V and Nb agglomerate and thicken due to a small amount of precipitate core, so that the pinning effect cannot be achieved sufficiently. (c) As a method to solve this problem, a production process that involves heat treatment of solid solution, cold rolling, and secondary heat treatment is effective.
    In the heat treatment of the initial solid solution, the alloying elements are sufficiently dissolved.
    In the next lamination step a, a distortion is given, while the amount of precipitated carbonitride core at the time of the next secondary heat treatment is increased, the carbonitrides are precipitated in a refined manner and the grains are made fine. (d) That is, in an alloy system that has an Mn content less than that of Patent Document 2, when cold rolling is carried out in an intermediate stage of two heat treatments, the precipitation of carbonitrides is stimulated and by refinement effect resulting from austenite grains and the precipitation strengthening action due to the carbonitride precipitation itself, a high resistance can be achieved, and also the resistance to hydrogen environment embrittlement can be accentuated.
    The present invention was completed based on the findings and their essences are austenitic stainless steels for high pressure hydrogen gas described in items (1) to (3) below. (1) An austenitic stainless steel for high pressure hydrogen gas consisting of a percentage by mass of C: 0.10% or less,
    Si: 1.0% or less, Mn: 3% or more less than 7%, Cr: 15 to 30%, Ni: 10% or more less than 17%, Al: 0.10% or less, N : 0.10 to 0.50%, and at least one type of V: 0.01 to 1.0% and Nb: 0.01 to 0.50%, the balance being Fe and impurities, where impurities, the content of P is 0.050% or less and the content is 0.050% or less, the tensile strength is 800 MPa or more, the number of grain size (ASTM E112) is No. 8 or more and carbonitrides alloys that have a maximum diameter of 50 to 1,000 nm are contained in the amount of 0.4 / um or more in the cross-sectional observation. (2) An austenitic stainless steel for high pressure hydrogen gas consisting, in percentage by mass, of C: 0.10% or less, Si: 1.0% or less, Mn: 3% or more less than 7 %, Cr: 15 to 30%, Ni: 10% or more to less than 17%, Al: 0.10% or less, N: 0.10 to 0.50%, and at least one type of V: 0.010 at 1.0% and Nb: 0.01 to 0.50%, and it additionally contains one or more types of elements from at least one group selected from a first group to a fourth group described below, the balance being Fe and impurities, where in impurities, the P content is 0.050% or less and the S content is 0.050% or less, the tensile strength is 800 MPa or more, the number of grain size (ASTM E112 ) is No. 8 oumaise and alloy carbonitrides that have a maximum diameter of 50 to 1,000 nm are contained in the amount of 0.4 / um or more in the cross-sectional observation.
    First group elements ... Mo: 0.3 to 3.0% and W: 0.3 to 6.0% Second group elements ... Ti: 0.001 to 0.5%, Zr: 0.001 to 0, 5%, Hf 0.001 to0.3% and Ta: 0.001 to 0.6% Third group elements ... B: 0.0001 to 0.020%, Cu: 0.3 to 5.0%, and Co: 0, 3 to 10.0% Fourth group elements ... Mg: 0.0001 to 0.0050%, Ca: 0.0001 to 0.0050%, La: 0.0001 to 0.20%, Ce: 0, 0001 to 0.20%, Y: 0.0001 to 0.40%, Sm: 0.0001 to 0.40%, Pr: 0.0001 to 0.40% and Nd: 0.0001 to 0.50%
    (3) Austenitic stainless steel for high pressure hydrogen gas, according to claim (1) or (2), in which austenitic stainless steel is subjected to heat treatment of a solid solution at a temperature of 1,000 to 1,200 ºC, after which it is subjected to afrio lamination in which the reduction in area is 20% or more, and subsequently it is again subjected to heat treatment in the temperature range of 900 ºC or more and less than the solution treatment temperature.
    Advantageous Effect of the Invention In accordance with the present invention, a high strength austenitic stainless steel can be provided which has a tensile strength of 800 MPa or more and is excellent in the embrittlement property of hydrogen environment in the region of composition of less than 7% Mn Description of the Modality The reasons for restricting the chemical composition and microstructure of a steel plate in the present invention are as follows: (A) Chemical composition of steel The operational advantages of each steel component and the preferential content of each component are described below.
    The symbol "%" that refers to the content of each element means "percentage by mass". C: 0.10% or less In the present invention, C (carbon) is not an element that is added positively.
    If the C content is greater than 0.10%, the carbides precipitate at the grain limits and have an adverse influence on the robustness and the like.
    Therefore, the C content is restricted to 0.10% or less.
    TeordeC is preferably 0.04% or less, more preferably 0.02% or less.
    The C content should be as low as possible.
    However, the extreme reduction in the C content content leads to an increase in the refinement cost, so that it is desirable to make the C content 0.001% or more in practical application.
    Si: 1.0% or less
    If Si (silicon) is contained in large quantities, Si forms an intermetallic compound with Ni, Cr, or the like, or promotes the formation of an intermetallic compound such as sigma phase, so that, in some cases, hot workability is decreased considerably. Therefore, the score is 1.0% or less. Preferably, the Si content is 0.5% or less. The Si content should be as low as possible. However, considering the cost of refinement, it is desirable to make the Si content 0.01% or more. Mn: 3% or more to less than 7% Mn (manganese) is an inexpensive austenite stabilizing element. In the steel of the present invention, due to an appropriate combination with Cr, Ni, N, and the like, Mn contributes to the enhancement of strength and the improvement in ductility and robustness. The present invention also aims to refine carbonitrides and make the grains fine. In the case where the amount of dissolved N is small, even if the steel is subjected to the process described below which consists of heat treatment of solid solution, cold rolling, and secondary heat treatment, carbonitrides having a density of sufficient number do not they can be precipitated, and it becomes difficult to accentuate the resistance due to the finer austenite grains. Therefore, 3% or more of Mn must be contained. If the Mn content is 7% or more, the technique described in Patent Document 2 can be applied. Therefore, in the present invention, the upper limit of the Mn content is less than 7%. For these reasons, the Mn content is specified to be 3% or more less than 7%. The preferential lower limit of the Mn content is 4%. In addition, the Mn content is effective when it is 6.5% or less, especially effective when it is 6.2% or less.
    Cr: 15 to 30% Cr (chromium) is an essential component because it is an element to ensure resistance to corrosion with a stainless steel. The Cr content must be 15% or more. However, if the Cr content is excessively high, coarse carbides such as M> 23Cs, which can decrease ductility and robustness, are easily formed in large quantities. Therefore, the appropriate Cr content is 15 to 30%. The Cr content is preferably 18 to 24%, more preferably 20 to 23.5%.
    Ni: 10% or more less than 17% Ni (nickel) is added as a stabilizing element for austenite. In the steel of the present invention, due to an appropriate combination with Cr, Mn, N and the like, Ni contributes to the increase in strength and the improvement in ductility and robustness. Therefore, the Ni content is 10% or more. However, if the Ni content is 17% or more, the saturation effect and the material cost increase. For these reasons, the appropriate Ni content is 10% or more to less than 17%. The Ni content is preferably 11 to 15%, more preferably 11.5 to 13.5%.
    Al: 0.10% or less Al (aluminum) is an important element as a deoxidizer. However, if the content of Al is greater than 0.10% and Al remains in large quantities, the formation of an intermetallic compound such as the sigma phase is promoted. Therefore, in order to obtain both the strength and the strength intended by the present invention, the Al content can be restricted to 0.10% or less. In order to achieve a reliable deoxidizing effect, the content of Al is desirably 0.001% or more. The Al content is preferably 0.05% or less, more preferably 0.03% or less. In this description, Al means the so-called "sol. Al (acid-soluble Al)".
    N: 0.10 to 0.50% N (nitrogen) is the most important solid solution strengthening element, and at the same time, in the present invention, it makes grains thin due to the formation of fine alloy carbonitrides, contributing to the accentuation of resistance. To use N to increase the resistance, 0.10% or more of N must be contained. However, if the N content is greater than 0.50%, thick nitrides are formed, and therefore the mechanical properties such as strength decrease. Therefore, the N content is 0.10 to 0.50%. The lower limit of the N content is preferably 0.20%, more preferably 0.30%. V: 0.01 to 1.0% and / or Nb: 0.01 to 0.50% V (vanadium) and Nb (niobium) are important elements in the steel of the present invention. To promote the formation of alloy carbonitrides and to contribute to the finer grains, either one or both of V and Nb must be combined. For these purposes, 0.01% or more of V and / or Nb needs to be combined. On the other hand, even if more than 1.0% V and / or more than 0.50% Nb are contained, the saturation effect and the material cost increase, so that the upper limits of the V content and the Nb content are 1.0% and 0.50%, respectively. The V content is preferably 0.10 to 0.30%, and the Nb content is preferably 0.15 to 0.28%. The inclusion of both V and Nb is more effective.
    P: 0.050% or less P (phosphorus), which is an impurity, is an element that has an adverse influence on the strength and similarity of steel. The P content is 0.050% or less, and is preferably as low as possible. The P content is preferably 0.025% or less, more preferably 0.018% or less.
    S: 0.050% or less S (sulfur), which is an impurity, is an element that, like P, has an adverse influence on the strength and similars of steel. The S content is 0.050% or less, and is preferably as low as possible. TeordeS is preferably 0.010% or less, more preferably 0.005% or less.
    The steel according to the present invention has the chemical composition described above, and in steel, the balance consists of Fe and impurities. The "impurities" in the "Fe and impurities" mean components that mixed due to various factors in the production process, including raw materials such as ore or waste, when steel is produced on an industrial scale, the components that are allowed to exist in the range so that they do not have an adverse influence on the present invention. The steel according to the present invention can contain, - as needed, one or more types of components selected from at least one group up to the four group described below. Below in this document, the components that belong to these groups are described. The elements that belong to the first group are Mo and W.
    These elements have a common operational advantage of stimulating the formation and stabilization of carbonitrides and contributing to the strengthening of a solid solution. The reasons for restricting the contents of these elements are as described below.
    Mo: 0.3 to 3.0%, W: 0.3 to 6.0% Mo (molybdenum) and W (tungsten) have an effect of forming carbonitrides and thereby making the grains thin, and also contributing to the strengthening of solid solution. Both of these elements achieve the effect when the content of each of these elements is 0.3% or more, so that these elements can be contained as needed. However, even if these elements are excessively contained, the effect saturates. Therefore, if these elements are contained, their contents should be as follows: Mo: 0.3 to 3.0%, and W: 0.3 to 6.0%.
    The elements that belong to the second group are Ti, Zr, Hf, and Ta. These elements have a common operational advantage in stimulating the formation of carbonitrides. Ti: 0.001 to 0.5%, Zr: 0.001 to 0.5%, Hf: 0.001 to 0.3% and Ta: 0.001 to 0.6% Ti (titanium), Zr (zirconium), Hf (hafnium), and Ta (tantalum), which, like V and Nb, have an effect of forming alloy carbonitrides and thereby making the grains thin, can be contained as needed. This effect can be achieved by containing 0.001% or more of each of these elements. However, even if these elements are excessively contained, the effect saturates. Therefore, the upper limits of the levels of these elements are respectively as follows: Ti: 0.5%, Zr: 0.5%, Hf: 0.3% and Ta: 0.6%. The upper limits of the contents of Ti and Zr are preferably 0.1%, more preferably 0.03%. The upper limit of the Hf content is preferably 0.08%, more preferably 0.02%. The upper limit of the content of Ta is preferably 0.4%, more preferably 0.3%. The elements belonging to the third group are B, Cu, and Co.
    These elements contribute to the accentuation of strength. The reasons for restricting the contents of these elements are as described below.
    B: 0.0001 to 0.020% B (boron), which makes the precipitates thin, and decreases the austenite grain diameter, while increasing the strength, can be contained as needed. The effect of this is achieved when the B content is 0.0001% or more. On the other hand, if the B content is excessive, a low melting point compound is formed and hot workability can be decreased. Therefore, the upper limit of the B content is 0.020%.
    Cu: 0.3 to 5.0%, Co: 0.3 to 10.0% Cu (copper) and Co (cobalt) are stabilizing elements of austenite, and contribute to the increase in strength due to the strengthening of solid solution. Therefore, 0.3% or more of either or both of these elements can be contained as needed. However, due to the balance between effect and material cost, the upper limits of the C Co levels are 5.0% and 10.0%, respectively.
    The elements that belong to the fourth group are Mg, Ca, La, Ce, Y, Sm, Pr, and Nd. These elements have a common action to prevent the solidification crack at the time of casting.
    Mg: 0.0001 to 0.0050%, Ca: 0.0001 to 0.0050%, La: 0.0001 to 0.20%, Ce: 0.0001 to 0.20%, Y: 0.0001 to 0.40%, Sm: 0.0001 to 0.40%, Pr:
    0.0001 to 0.40% and Nd: 0.0001 to 0.50% Mg (magnesium) and Ca (calcium), and La (lanthanum), Ce (cerium), Y (yttrium), Sm (samarium), Pr (praseodymium), and Nd (neodymium) among the transition metals have an action to prevent the solidification crack at the time of casting.
    Therefore, one or more types of these elements can be contained as needed.
    This effect can be achieved by containing 0.0001% or more of each of these elements.
    On the other hand, if these elements are excessively contained, hot workability decreases.
    Therefore, the upper limits of the levels of these elements are as follows: Mg and Ca: 0.0050%, La and Ce: 0.20%, Y, Sm and Pr: 0.40% and Nd: 0.50%. (B) Steel microstructure The nitrogen used in the present invention is effective in carrying out the strengthening of the solid solution, but it has an action so that the distortion at the moment of deformation is localized, decreasing the stacking failure energy, and the durability against the embrittlement of hydrogen environment is decreased.
    However, by decreasing the grain diameter, both the increase in resistance to 800 MPa or more and the prevention of hydrogen embrittlement are enabled.
    In order to avoid embrittlement of the hydrogen environment, the grain size number (ASTM E112) is No. 8 or more, preferably No. 9 or more, and most preferably No. 10 or more.
    In order to make the grains thin, pinning using alloy carbonitrides is effective.
    To achieve this effect, alloy carbonitrides that are 50 to 1,000 nm in size need to be contained in the amount of 0.4 / um or more in the cross-sectional observation.
    These alloy carbonitrides are those that contain Cr, V, Nb, Mo, W, Ta, and the like as main components, and have a crystalline Z-phase structure, that is, Cr (Nb, V) (C, N) or of the MX type (M: Cr, V, Nb, Mo, W, Ta, and the like, X: C, N). The alloy carbonitrides in the present invention are carbonitrides that barely contain Fe. Even if Fe is contained, the amount of Fe is 1% atom or less. In addition, the carbonitrides in the present invention include those in which the C (carbon) content is extremely low, i.e., those consisting of nitrides. (C) Production method In order to make fine grains as described in (B) and to precipitate fine alloy carbonitrides that have a desired number density, the common method cannot be used. However, the steel of the present invention can be produced by successively undergoing the heat treatment of solid solution, cold rolling and secondary heat treatment described below.
    The first heat treatment of a solid solution must be carried out at a temperature of 1,000 ºC or more, preferably 1,100 ºC or more, to dissolve the alloy elements sufficiently. However, if the solution heat treatment temperature is greater than 1,200 "ºC, the grains are extremely thickened. Therefore, the upper limit of the heat treatment temperature of solid solution is 1,200 ºC. Below in this document, for convenience, the heat treatment temperature in the solid solution heat treatment is referred to as a "T1 temperature".
    In the heat treatment of solid solution according to the present invention, solution treatment of a degree necessary to precipitate carbonitrides in the subsequent secondary heat treatment should only be carried out and all elements forming carbonitride need not necessarily be dissolved. The steel material that has been subjected to heat treatment of solid solution is preferably cooled rapidly from the heat treatment temperature of solid solution. In this case, water cooling (immersion or shower water cooling) is preferred.
    In addition, in relation to the heat treatment of solid solution,
    an independent solid solution heat treatment step does not necessarily have to be provided. By performing rapid cooling after a hot work process such as hot extrusion, the equivalent effect can be achieved. For example, rapid cooling should only be performed after hot extrusion at about 1,150 ºC.
    In addition, in order to increase the amount of carbonite precipitate core, cold rolling is carried out at a cold rolling rate so that the area reduction is 20% or more. The upper limit of the cold rolling ratio is not particularly restricted.
    However, considering the working rate at the time when a common member is subjected to cold rolling, 90% or less of the cold rolling ratio is preferred. Finally, in order to remove the distortion caused by cold rolling and to make the grains fine by precipitating fine carbonitrides, the secondary heat treatment is carried out at a temperature lower than the temperature T1. Below in this document, for convenience, the heat treatment temperature in the secondary heat treatment is referred to as a "T2 temperature".
    Temperature T2 is lower than temperature T1. In order to make the grains thin, the upper temperature limit T2 is preferably set to [treatment temperature T1 - 20 ºC], and most preferably set to [treatment temperature T1 - 50 ºC]. Specifically, the upper temperature limit T2 is preferably set to 1,150 ºC, and more preferably made 1,080 ºC. On the other hand, the lower limit of the T2 temperature is 900 ºC because if the T2 temperature is less than 900 ºC, coarse Cr carbides are formed, and therefore the microstructure becomes non-uniform.
    Examples In the following, the effects of the present invention are explained based on the examples.
    Fifty kilograms of each stainless steel that has the chemical compositions given in Table 1 was vacuum cast and hot forged to form a block that is 40 to 60 mm thick. Table 1 Wounds the LS So of REA of [Steel | CC TS TM TT PT ENO VI No Fans) [A | 0020 | 0.40] 4.55 | 0.010] 0.001 | 12.25] 22.50 | 0.20 | 0.20 | 0.020 | aa PúÁNEIsIs: «cdiB | 8 | 0.010 | 0.42] 5.50 | 0.015 | 0.001 | 13.45 | 20.58 | 0.28 [0.15510015 as ris un nn | C | 0.008 | 0.43 | 460 | 0.009 | <0.001 | 12.55 | 22.10 [0.12 [0.28 [0.017 | 630 úúÂÚsIsisll: | D [0005048] 412 [0.015] 0.001 | 12.19 | 18.31 | 0.08 0.05 oo oa NÂNÚRIiIi] iriBrii: I :. uu | E [0.015 [045/5580 0.018 20,001 11,22 / 18,55) - JO21 / 0Nis | 0238] À ÀÀÀÂúôm | À] * "& MAO [| F [0.005 | 0.40 | 5.10 | 0.008] 0.002 | 14.85 | 23.75 [048] - / oo25 | gas UNS | G | 0.050 [0 , 35] 6,85 | 0,020 | <0,001 | 10,25 | 15,15 | - foasfooms fire ÂÚÂÚÚAIRrIsirirIBi: E EN | H [0,055 0,36] 4,51 | 0,009 | 0,001 | 10,85 | 17,85 | 0.05 0.22 hollow oa PÚÁÚÂÚÂÚ |] ss = uis;: l «>« ”> & rilisi:« = l = IlIli: r li | 1 / 0.033 / 065] 3.10 [0.015] 0.003 | 16, 82 | 28.85 [0.65] - 0045] aa NNNÂÂÂ | | J | 0.025 | 045 | 475 | 0.008 | 0.001 | 12.20 | 22.10 [0.21 | 0.10 [0078 oa ÂÚÂÚÂN Aa o | K 0021 [043 | 455 | 0.010] 0.001 | 12.55 | 22.95 | 0.18 | 0.20 | 0.020 | 0.30 | Ti: 0.022 | L | o009 | 043 | 5.10 | 0.012 | <0.001 | 11.80 | 20.22 | 0.10 | 0.15 | 0.028 oa PÂÚÂÚÂÚÂÚÔNÃN so ggaa & | M [0019046] 5.01 | 0.009] 0.001 [12.05] 2315 [019 021/0019 032 To the case is | N [0021 | 048 | 485 | 0.008] 0.001 | 13.20 | 21.84 [028 009 0021 030 -ÀÀÚ —JSaçoots [| O [0015 | 0.36 | 495 | 0.014 | <0.001 | 12.96 | 22.01 | 0.22 | 0.20 (0020 oo Ne a [| P [0019 [044] 5.05 | 0.015] 0.001 | 11.85 | 22.55 | 0.18 | 0.19 [0.022 | 0.31 | Mo: 1.95, Zr: 0.025% [a | 0: 035 | 0.49 | 5.52 | 0.008 | 0.002 [13.20 | 2301 [012/020 [/ 0.028 / 030] W401.8: 0.0055 | <& | R | 0022 [0.44 | 488 | 0.009 | 0.001 | 12.05 | 2220 | 0.20 | 0.15 | 0.017 | 0.33 | Mo: 2.05, Mg: 0.0025 o | S | 0021 / 0.43] 455 [0.010 | 0.001 | 12.55 | 22.95 | 0.18 | 0.10 [0.020 | 0.30 | Ta: 0.20, Cu: 4.5 | T | oo15 045] 4.89 | 0.009 | 0.002 | 12.09 | 21.06 | 0.19 | 0.20 [0.025 | 0.30 | Ti: 0.015, Ca: 0.0025 | U | 0011 [0.44] 4.86 [0.070 | 0.001 | 12.08 | 20.85 | 0.15 | 0.19 [0.020 | 0.38 | B: 0.0015, Mg: 0.0041 | V | 0o015 [045] 5.098 [0.072] 0.001 | 12.04] 21.04 | 0.19 | 0.20 [0.021 | 0.39 | Cu: 4.8, Ca: 0.0035 [| w | 0009 | 048] 4.86 | 0.008 | <0.001 | 12.07 | 20.96 | 0.26 | 0.09 [0.019 | 0.36 | Mo: 2.15, Ti: 0.010, B: 0.0025 0.010 | 0.47 | 4.99 | 0.011 | 0.001 [12.51 | 21.48 | 0.21 [0.15 | 0.015 | 0.32 | Mo: 1.95, Ti: 0.015, Cu: 3.7 | y Joot6 | 047] 5.21 0.011 | 0.001 | 12.25 | 21.59 [0.24 [0.18 [0018 | 0.30 | Mo: 2.15, Zr: 0.045, Ca: 0.0020 | z | 0.020 / 0.49] 5.56 [0.012] 0.002 | 13.16 | 23.08 | 0.27 | 0.20 [0.018 | 0.33 | Ta: 0.21, Cu: 4.2, Mg: 0.0035 | 1 | o015 | 046] 4.95 | 0.015 | <0.001 | 12.95 | 22.98 | 0.23 | 0.14 [0.016 | 0.30 | Mo: 2.85, Ti: 0.010, Cu: 3.5, La: 0.10 | 2 | 0010 [041] 5.25 [0.009 | 0.001 | 13.01 | 21.91 [0.21 | 0.15 [0.021 | 0.31 | Mo: 3.01, Ti: 0.009, Cu: 3.0, Y: 0.11 | 3 [0011 045] 491 | 0.008 | <0.001 | 13.25 | 22.05 | 0.20 | 0.13 [0.020 | 0.30 | Mo: 2.95, Ti: 0.012, Cu: 3.4, Pr: 0.11 | 4 10.035 10.44] 2.05 "| 0.008 | 0.001 | 12.51 | 21.95 [023] Moore Toae OO | —3 | -0.009 | 0.46 | 5.01 | 0.007 | 0.001 | 9.02º | 22.10 025] Tools] 9a ———— | | o012 [0.49] 5.22 | 0.072 | 0.001 | 12.36 | 30.557 0.23] "oo ONT« and 7 [0.009 5.01 | 0.009 12.14 | 21.96 [0.16 u &
    E 8 o 8 <* shows the scope of the steel of the invention. Subsequently, the block was hot-rolled to a predetermined thickness and underwent a one-hour solid solution heat treatment, cold rolling and one-hour secondary heat treatment, while an 8 mm thick slab material was formed . In Table 2, the heat treatment temperature of solid solution (temperature T1) of each test number is expressed by T1 (ºC), and the secondary heat treatment temperature (temperature T2) of it is expressed by T2 (ºC). The cold rolling ratio of each test No. is also shown in Table 2. Table 2 Test | Steel IT Ratio T2 * of TS Number Break of No. Lamination Size | Grain relative (Co) afrium (ºC) carbonitrides | (x10 / 25um ) | (MPa) | elongation (%) ETA ee As Tem mo | as Tee and | 2 DA [100 47 "5000] the [OA VT & Es A LT are Ta in the TAS e] 8 a | Ac 110 / so [71050/105 | ss [os [| 101" sa Ro os TT ar [SS TST and Fe A tw a more A py uv | El A Timm rr eos to live 028 1 68) 2nd | Be B | 100/2 [9700 103 [29 (66) &%) ES re [10] 29 3406) 105 | 27 [sos [| 8 Lo pie> 40) 3 | 2 (e TE | | | E 1100 | 3 Too NA | 3 Te E ER EF 1100 256 [1000] 103 | "es [e Is e 1100/23 Tron RnryT 2 Te ss | et HEI. 29 Emo rivers DB [80 ] 3) Ra TI me Ss oo ros [| 6 | ei 8 pe a 100 [RS ana oz TC ep TT im.
    Go K | Too Rs JA os os Tal mm e [8 E do | as Too | the Te TT] Tso8 | s8) Es EM iDo os ooo Toa ar | Tee 29 EN ao [os TA O00 1 oo o eBis in [21 o years as TO BBCs and re Pp o) Rs Toon [os (os] o | Es oo OS TON TA Ao BB | as 2nd CR 1100 os Jos] 024 [2 eos | se 26 1100 | ae 1 Is a - ES —e— 1 26 | T | 1100] om o2 Ta TB [1 ss | E o To T Os 7000 2 | 8 Jos | o Es [vs 350) 2 | dev e) Law 100 Os oo os [Uses and es | [30 [XT] 35 To | os | The “Teos 108 Es Tr os Os om [es [| TOM and 19. Es zZ To TOS rom | os [SC Tr es Less LIT TOS ooo os [SS Tn | and | = 12 ooo at 50 | 109 | > JT] | Es 3 Too) 3 | eo rt oo [OT [ap | 19) 28 CA aaa Ao on | rs OSS year | 68 or A 65 Tao oa or os Te | 6: | sa ro O mo er os Tee ss, | 39 | A | ST oo AR (TS Oss 70] à é A A | 300] Os To] Tae TT a as. Sn) ECA oo Oo Pal Ts | the leon 7 | ss Ea a from URB oo 7a | O oa BN Es nas | 5 ro os Too ans Ooo an ss "ae io | os 190 [os | 8“ Tamil ae -) LEFT) Os “Mon Tr) 0 Tr nn |
    * shows the scope of the steel of the invention.
    ** shows the scope of the method of the invention.
    One specimen was sampled and incorporated with a resin so that the cross-section perpendicular to the lamination direction of the plate material can be observed and after electrolytic textualization, the number of grain size (in accordance with ASTM E112) was measured. In addition, similarly, using a resin incorporating material in the cross-sectional direction, the number of precipitates was measured by observation under an electron microscope using an extraction replica method. A region of 25 um was observed at a magnification of x10,000 in ten visual fields and precipitates having a size of 50 to 1,000 nm were measured. The precipitates measured in the examples were phase Z carbonitrides of rhombic structure containing similar Cr, V, Nb, C, Ne, or MX type of tetragonal structure containing similar Cr, Nb, V, C, Ne.
    A round bar tensile test specimen that has a diameter of 3 mm in its parallel part was sampled in the longitudinal direction of the plate material and a tensile test was conducted at a tension rate of 3 x 10 $ / s in the atmosphere at normal temperature or at 85 MPa high pressure hydrogen gas at normal temperature to measure tensile strength (TS) and elongation at break. Since hydrogen has a notable influence on the decrease in ductility, the ratio of elongation at break in hydrogen to elongation at break in the atmosphere has been made a relative elongation at break and has been interpreted as if the relative elongation at break is 80% or more, preferably 90% or more, the decrease in ductility caused by hydrogen is slight and the resistance to hydrogen embrittlement is excellent.
    The stress rate of 3 x 10 $ / s in the tensile test described above is considerably lower than the stress rate of 10º / s in the tensile test in the high pressure hydrogen gas environment, which was used in conventional documents. The reason for this is that in the recent assessment standards on durability assessment against hydrogen environment embrittlement, the assessment test at a very low stress rate, in which the susceptibility to hydrogen environment embrittlement of austenitic stainless steel becomes larger, it is recommended.
    Table 2 summarized the number of grain size, the number of carbonitrides, tensile strength (TS), and the relative elongation at break of the steel being tested. Tests No. 1 to 35 are exemplary embodiments of the present invention, in which the grain size number was No. 8 or more, a sufficient number of carbonitrides were precipitated, the TS was 800 MPa or more, and the elongation at break relative value was also 80% or more, with sufficient resistance to hydrogen embrittlement being achieved.
    Tests No. 36 to 41 are comparative examples. In the No. 36 Test, the heat treatment temperature of solid T1 solution was very high, the grains were thickened and the resistance to hydrogen embrittlement was poor. In Test No. 37, the heat treatment temperature of solid T1 solution was very low, the density of number of carbonitrides was low, the grains were thickened and the resistance to hydrogen embrittlement was poor. In Tests No. 38 and 39, the cold rolling ratio was low, the number of carbonitride precipitation was insufficient, the grains were thickened and the resistance to hydrogen embrittlement was poor. In Test No. 40, the secondary heat treatment temperature T2 was very high, the grains were thickened and the resistance to hydrogen embrittlement was poor. In Test No. 41, the heat treatment temperature of the final solid solution T2 was very low, the density of number of carbonitrides was low, the grains were thickened and the resistance to hydrogen embrittlement was poor.
    Tests Nos. 42 to 45 are comparative examples, in which the chemical composition of material steel was outside the range of the present invention.
    In Test No. 42, the Mn content was very low, and as a result N (nitrogen) could not be contained sufficiently, the grains were thickened, the resistance was low and the resistance to embrittlement of the hydrogen environment was poor.
    In Test No. 43, the Ni content was low, ô ferrite was formed and the resistance to embrittlement of hydrogen environment was poor.
    In Test No. 44, the Cr content was high, coarse Cr carbides were formed and the resistance to hydrogen embrittlement was poor.
    In Test No. 45, the N (nitrogen) content was low, the grains were thickened, the resistance was low and the resistance to embrittlement of the hydrogen environment was poor.
    Industrial Applicability
    As described above, according to the present invention, even an austenitic stainless steel that contains less than 7% Mn can become a high-strength steel with excellent hydrogen environment embrittlement property by interposing a cold rolling step between two heat treatments, and therefore can be used for pipes and containers for high pressure hydrogen gas.
    权利要求:
    Claims (3)
    [1]
    1. Austenitic stainless steel for high pressure hydrogen gas CHARACTERIZED by the fact that it consists, in percentage by mass, of C: 0.10% or less, Si: 1.0% or less, Mn: 3% or more less than 7%, Cr: 15 to 30%, Ni: 10% or more to less than 17%, Al: 0.10% or less, N: 0.10 to 0.50%, and at least one type of V: 0 , 01 to 1.0% and Nb: 0.01 to 0.50%, with the balance being Fe and impurities, where in impurities, the P content is 0.050% or less and the S content is 0.050% or less, the tensile strength is 800 MPa or more, the grain size number (ASTM E112) is No. 8 or more and —carbon alloys that have a maximum diameter of 50 to 1,000 nm are contained in the quantity 0.4 / one or more in the cross-sectional observation.
    [2]
    2. Austenitic stainless steel for high pressure hydrogen gas CHARACTERIZED by the fact that it consists, in percentage by mass, of C: 0.10% or less, Si: 1.0% or less, Mn: 3% or more less than 7%, Cr: 15 to 30%, Ni: 10% or more to less than 17%, Al: 0.10% or less, N: 0.10 to 0.50%, and at least one type of V: 0.010 at 1.0% and Nb: 0.01 to 0.50%, and it additionally contains one or more types of elements from at least one group selected from a first group to a fourth group described below, the balance being Fe and impurities, where in impurities, the P content is —0.050% or less and the S content is 0.050% or less, the tensile strength is 800 MPa or more, the grain size number (ASTM E112) is No. 8 or more and alloy carbonitrides that have a maximum diameter of 50 to 1,000 nm are contained in the amount of 0.4 / um or more in the cross-sectional observation. First group elements ... Mo: 0.3 to 3.0% and W: 0.3 to 6.0% Second group elements ... Ti: 0.001 to 0.5%, Zr: 0.001 to 0, 5%, Hf: 0.001 to 0.3% and Ta: 0.001 to 0.6% Third group elements ... B: 0.0001 to 0.020%, Cu: 03a 5.0%, and Co: 0.3 at 10.0% Fourth group elements ... Mg: 0.0001 to 0.0050%, Ca: 0.0001 to 0.0050%, La: 0.0001 to 0.20%, Ce: 0.0001 to 0.20%, Y: 0.0001 to 0.40%, Sm: 0.0001 to 0.40%, Pr: 0.0001 to 0.40% and Nd: 0.0001 to 0.50%
    [3]
    3. Austenitic stainless steel for high pressure hydrogen gas, according to claim 1 or 2, CHARACTERIZED by the fact that austenitic stainless steel is subjected to heat treatment of solid solution at a temperature of 1,000 to 1,200 ºC, after which it is subjected to cold lamination in which the reduction in area is 20% or more, and subsequently it is again subjected to heat treatment in the temperature range of 900 ºC or more and less than the solution treatment temperature.
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    同族专利:
    公开号 | 公开日
    AU2012234641B2|2015-01-29|
    EP2692886B1|2019-05-08|
    WO2012132992A1|2012-10-04|
    DK2692886T3|2019-08-12|
    CN103476959B|2016-03-23|
    EP2692886B8|2019-07-10|
    US20140017111A1|2014-01-16|
    JP5131794B2|2013-01-30|
    ES2735299T3|2019-12-17|
    CA2824463A1|2012-10-04|
    US10266909B2|2019-04-23|
    KR101543938B1|2015-08-11|
    JPWO2012132992A1|2014-07-28|
    CA2824463C|2016-12-13|
    AU2012234641A1|2013-08-01|
    EP2692886A4|2015-11-18|
    KR20130121981A|2013-11-06|
    US10260125B2|2019-04-16|
    CN103476959A|2013-12-25|
    EP2692886A1|2014-02-05|
    US20160304983A1|2016-10-20|
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    法律状态:
    2021-04-13| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2021-04-20| B25D| Requested change of name of applicant approved|Owner name: NIPPON STEEL CORPORATION (JP) |
    2021-05-18| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2021-09-21| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|
    2021-12-14| B350| Update of information on the portal [chapter 15.35 patent gazette]|
    2022-02-15| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    优先权:
    申请号 | 申请日 | 专利标题
    JP2011070045|2011-03-28|
    JP2011-070045|2011-03-28|
    PCT/JP2012/057001|WO2012132992A1|2011-03-28|2012-03-19|High-strength austenitic stainless steel for high-pressure hydrogen gas|
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