EP3524705B1 - Alliage à base de ni-cr-fe - Google Patents

Alliage à base de ni-cr-fe Download PDF

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EP3524705B1
EP3524705B1 EP17858416.5A EP17858416A EP3524705B1 EP 3524705 B1 EP3524705 B1 EP 3524705B1 EP 17858416 A EP17858416 A EP 17858416A EP 3524705 B1 EP3524705 B1 EP 3524705B1
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content
alloy
rem
nicrfe
phase
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EP3524705A1 (fr
EP3524705A4 (fr
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Hirokazu Okada
Tomoaki Hamaguchi
Shinnosuke KURIHARA
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Nippon Steel Corp
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese

Definitions

  • the present invention relates to an austenitic heat resistant alloy, and more specifically a NiCrFe alloy.
  • facilities such as thermal power generation boilers and chemical plants are operated in high temperature environments (such as 400 to 800°C) and, in addition, they are brought into contact with process fluids including sulfides and/or chlorides. Therefore, materials to be used in such facilities require their creep strength and corrosion resistance at high temperatures.
  • Examples of the material for use in such facilities include 18-8 stainless steel such as SUS304H, SUS316H, SUS321H, and SUS347H, and NiCrFe alloys represented by Alloy 800H, which is specified as NCF800H by the JIS standard.
  • a NiCrFe alloy excels in corrosion resistance and high temperature strength compared to an 18-8 stainless steel. Further, a NiCrFe alloy excels in economic efficiency compared to a Ni-base alloy represented by Alloy617. Therefore, NiCrFe alloys are widely used in regions of severe use environments.
  • Patent Literature 1 Japanese Patent Application Publication No. 2013-227644
  • Patent Literature 2 Japanese Patent Application Publication No. 06-264169
  • Patent Literature 3 Japanese Patent Application Publication No. 2002-256398
  • Patent Literature 4 Japanese Patent Application Publication No. 08-13104
  • a heat resistant and corrosion resistant alloy disclosed in Patent Literature 2 consists of, in weight%, 55 to 65% of Nickel, 19 to 25% of Chromium, 1 to 4.5% of Aluminum, 0.045 to 0.3% of Yttrium, 0.15 to 1% of Titan, 0.005 to 0.5% of Carbon, 0.1 to 1.5% of Silicon, not more than 1% of Manganese, a total of 0.005% of at least one element selected from the group consisting of Magnesium, Calcium, and Cerium, a total of less than 0.5% of Magnesium and Calcium, less than 1% of Cerium, 0.0001 to 0.1% of Boron, not more than 0.5% of Zirconium, 0.0001 to 0.2% of Nitrogen, and not more than 10% of Cobalt, with the balance being Fe and accompanying impurities.
  • An austenitic alloy disclosed in Patent Literature 3 contains, in mass%, C: 0.01 to 0.1%, Mn: 0.05 to 2%, Cr: 19 to 26%, and Ni: 10 to 35%, with the Si content satisfying a formula of 0.01 ⁇ Si ⁇ (Cr + 0.15 ⁇ Ni - 18)/10.
  • a heat resistant alloy disclosed in Patent Literature 4 consists of, in weight%, C: 0.02 to 0.15%, Si: 0.70 to 3.00%, Mn: not more than 0.50%, Ni: 30.0 to 40.0%, Cr: 18.0 to 25.0%, Al: 0.50 to 2.00%, and Ti: 0.10 to 1.00%, with the balance being Fe and inevitable impurities. Further, also Patent Application Publication US2010/034690 discloses an austenitic NiCrFe-alloy.
  • Non Patent Literature 1 Hans van Wortel: “Control of Relaxation Cracking in Austenitic High Temperature Components", CORROSION2007 (2007), NACE, Paper No.07423
  • the austenitic heat resistant alloy disclosed in Patent Literature 1 controls the formation of Laves phase by specifying the contents of W, Mo, Nb, and Ti, thereby improving creep strength and toughness.
  • the heat resistant and corrosion resistant alloy disclosed in Patent Literature 2 improves high-temperature oxidation resistance by causing ⁇ ' to be precipitated during creep.
  • the austenitic alloy disclosed in Patent Literature 3 improves carburizing properties by suppressing exfoliation of the oxide film dominantly composed of Cr 2 O 3 and formed on the material surface.
  • the heat resistant alloy disclosed in Patent Literature 4 contains a specific amount of Cr, a reduced amount of Mn, and a fixed amount of Si, thereby making it possible to obtain excellent oxidation resistance even in a case in which the Ni content is reduced.
  • Non Patent Literature 1 discloses that a NiCrFe alloy has a high susceptibility to stress relaxation cracking. This means that a NiCrFe alloy requires stress relief heat treatment, after working, for a bent part and welded part, in which residual stress is present. Therefore, a NiCrFe alloy requires not only excellent creep strength but also excellent stress relaxation cracking resistance.
  • An objective of the present invention is to provide a NiCrFe alloy which excels in creep strength and stress relaxation cracking resistance.
  • a NiCrFe alloy according to the present invention has a chemical composition consisting of, in mass%, C: 0.03 to 0.15%, Si: not more than 1.00%, Mn: not more than 2.00%, P: not more than 0.040%, S: not more than 0.0050%, Cr: 18.0 to 25.0%, Ni: 25.0 to 40.0%, Ti: 0.10 to 1.60%, Al: 0.05 to 1.00%, N: not more than 0.020%, O: not more than 0.008%, rare earth metal (REM): 0.001 to 0.100%, B: 0 to 0.010%, Ca: 0 to 0.010%, Mg: 0 to 0.010%, V: 0 to 0.5%, Nb: 0 to 1.0%, Ta: 0 to 1.0%, Hf: 0 to 1.0%, Mo: 0 to 1.0%, W: 0 to 2.0%, Co: 0 to 3.0%, and Cu: 0 to 3.0%, with the balance being Fe and impurities, the chemical composition satisfying Formulae (1) to (3)
  • a NiCrFe alloy according to the present invention excels in creep strength and stress relaxation cracking resistance.
  • FIG. 1 is a diagram to show a relation between fn2 of each Reference mark of Examples, and a sum (mass%) of ⁇ ' and ⁇ phase after aging treatment.
  • the present inventors have conducted detailed study on the creep strength and the stress relaxation cracking resistance of NiCrFe alloys. As a result, the present inventors have obtained the following findings.
  • adjusting the content of REM to be an appropriate amount will allow improving the stress relaxation cracking resistance of the NiCrFe alloy.
  • REM combines with S and is also likely to combine with O easily. Therefore, to immobilize S by REM, the REM content should be adjusted while the amount of REM that combines with O is taken into consideration.
  • ⁇ [REM/(A(REM))] is substituted by an addition sum of values which are obtained by dividing each REM content (mass%) contained in the NiCrFe alloy by the atomic weight of the REM.
  • fn3 ⁇ [REM/(A(REM))] - S/32 - 2/3•O/16.
  • REM is a generic name of a total of 17 elements of Sc, Y, and lanthanoids.
  • fn3 is not less than 0, REM can sufficiently immobilize S as inclusions, thereby improving the stress relaxation cracking resistance.
  • the NiCrFe alloy according to the present invention which has been completed based on the above described findings, has a chemical composition consisting of, in mass%, C: 0.03 to 0.15%, Si: not more than 1.00%, Mn: not more than 2.00%, P: not more than 0.040%, S: not more than 0.0050%, Cr: 18.0 to 25.0%, Ni: 25.0 to 40.0%, Ti: 0.10 to 1.60%, Al: 0.05 to 1.00%, N: not more than 0.020%, O: not more than 0.008%, rare earth metal (REM): 0.001 to 0.100%, B: 0 to 0.010%, Ca: 0 to 0.010%, Mg: 0 to 0.010%, V: 0 to 0.5%, Nb: 0 to 1.0%, Ta: 0 to 1.0%, Hf: 0 to 1.0%, Mo: 0 to 1.0%, W: 0 to 2.0%, Co: 0 to 3.0%, and Cu: 0 to 3.0%, with the balance being Fe and im
  • the above described chemical composition may contain B: 0.0001 to 0.010%.
  • the above described chemical composition may contain one or two types selected from the group consisting of Ca: 0.0001 to 0.010%, and Mg: 0.0001 to 0.010%.
  • the above described chemical composition may contain one or more types selected from the group consisting of V: 0.01 to 0.5%, Nb: 0.01 to 1.0%, Ta: 0.01 to 1.0%, and Hf: 0.01 to 1.0%.
  • the above described chemical composition may contain one or more types selected from the group consisting of Mo: 0.01 to 1.0%, W: 0.01 to 2.0%, Co: 0.01 to 3.0%, and Cu: 0.01 to 3.0%.
  • the NiCrFe alloy according to the present invention has excellent creep strength and excellent stress relaxation cracking resistance. To be more specific, the NiCrFe alloy will not rupture for 300 or more hours even if it is subjected to tensile strain of 10% at a strain rate of 0.05 min -1 and is kept as is under air atmosphere of 650°C after being subjected to cold rolling at a reduction of area of 20%.
  • the chemical composition of NiCrFe alloy of the present invention contains the following elements.
  • C content is 0.03 to 0.15%.
  • the lower limit of the C content is preferably 0.04%, more preferably more than 0.04%, and further preferably 0.05%, and further preferably 0.06%.
  • the upper limit of the C content is preferably 0.12%, and more preferably 0.10%.
  • Si Silicon
  • Si is inevitably contained. Si deoxidizes the alloy, and improves the corrosion resistance and oxidation resistance at high temperatures of the alloy. However, when the Si content is too high, the stability of austenite deteriorates, and toughness and creep strength of the alloy decrease. Therefore, the Si content is not more than 1.00%.
  • the upper limit of the Si content is preferably 0.80%, more preferably 0.60%, and further preferably less than 0.60%. Excessive reduction of the Si content deteriorates deoxidization effect, thus deteriorating the corrosion resistance and oxidization resistance at high temperatures of the alloy. And further, the production cost is significantly increased. Therefore, the lower limit of the Si content is preferably 0.02%, and more preferably 0.05%.
  • Mn Manganese
  • the upper limit of the Mn content is preferably 1.80%, and more preferably 1.50%. Excessive reduction of the Mn content deteriorates the deoxidization effect and stabilization of austenite, and further causes significant increase of the production cost. Therefore, the lower limit of the Mn content is preferably 0.10%, more preferably 0.30%, and further preferably more than 0.50%.
  • Phosphorous (P) is an impurity. P deteriorates hot workability and weldability of the alloy, and also deteriorates creep ductility of the alloy after long hours of usage. Therefore, the P content is not more than 0.040%.
  • the upper limit of the P content is preferably 0.035%, and more preferably 0.030%.
  • the P content is preferably as low as possible. However, excessive reduction of the P content will increase the production cost. Therefore, the lower limit of the P content is preferably 0.0005%, and more preferably 0.0008%.
  • S Sulfur
  • S is an impurity. S deteriorates the stress relaxation cracking resistance of the alloy, and also deteriorates the hot workability, weldability, and creep ductility of the alloy. Therefore, the S content is not more than 0.0050%.
  • the upper limit of the S content is preferably 0.0030%.
  • the S content is preferably as low as possible. However, excessive reduction of the S content will increase the production cost. Therefore, the lower limit of the S content is preferably 0.0002%, and more preferably 0.0003%.
  • Chromium (Cr) improves the oxidation resistance and corrosion resistance at high temperatures of the alloy. When the Cr content is too low, these effects cannot be obtained. On the other hand, when the Cr content is too high, the stability of austenite at high temperatures deteriorates and the creep strength of the alloy decreases. Therefore, the Cr content is 18.0 to 25.0%.
  • the lower limit of the Cr content is preferably 18.5%, and more preferably 19.0%.
  • the upper limit of the Cr content is preferably 24.5%, and more preferably 24.0%.
  • the lower limit of the Ni content is preferably 26.0%, and more preferably 27.0%.
  • the upper limit of the Ni content is preferably 37.0%, and more preferably 35.0%.
  • Titanium (Ti) combines with Ni to form ⁇ '. Further, Ti combines with C to form TiC, thereby increasing the creep strength and tensile strength of the alloy at high temperatures. When the Ti content is too low, such effects cannot be obtained. On the other hand, when the Ti content is too high, ⁇ ' precipitates excessively, thereby deteriorating the stress relaxation cracking resistance of the alloy. Therefore, the Ti content is 0.10 to 1.60%.
  • the lower limit of the Ti content is preferably 0.20%, more preferably 0.30%, and further preferably more than 0.60%.
  • the upper limit of the Ti content is preferably 1.50%, more preferably less than 1.50%, and further preferably 1.40%.
  • the lower limit of the Al content is preferably 0.08%, and more preferably 0.10%.
  • the upper limit of the Al content is preferably 0.90%, and more preferably 0.80%.
  • N Nitrogen
  • the upper limit of the N content is preferably 0.017%, and more preferably 0.015%.
  • the N content is preferably as low as possible. However, excessive reduction thereof will increase production cost. Therefore, the lower limit of the N content is preferably 0.002%, and more preferably 0.004%.
  • Oxygen (O) is an impurity. Oxygen deteriorates the hot workability of the alloy, and also deteriorates the toughness and ductility of the alloy. Therefore, the O content is not more than 0.008%.
  • the upper limit of the O content is preferably 0.006%, and more preferably 0.005%.
  • the O content is preferably as low as possible. However, excessive reduction thereof will increase the production cost. Therefore, the lower limit of the O content is preferably 0.0005%, and more preferably 0.0008%.
  • Rare earth metal forms a compound with S, thereby decreasing the content of S which has dissolved into the matrix, and improving the stress relaxation cracking resistance of the alloy. Further, REM improves the hot workability and oxidization resistance of the alloy. When the REM content is too low, these effects cannot be obtained. On the other hand, when the REM content is too high, the hot workability and weldability of the alloy will deteriorate. Therefore, the REM content is 0.001 to 0.100%.
  • the lower limit of the REM content is preferably 0.003%, and more preferably 0.005%.
  • the upper limit of the REM content is preferably 0.090%, and more preferably 0.080%.
  • REM is a generic name of a total of 17 elements of Sc, Y, and lanthanoids, and the REM content refers to a total content of one or more elements of REM. Moreover, REM is generally contained in misch metal. For that reason, REM may be added to molten metal as misch metal, and may be adjusted such that the REM content is within the above described range.
  • the balance of the chemical composition of the NiCrFe alloy according to the present invention consists of Fe and impurities.
  • impurity means an element which is introduced from ores and scraps as the raw material, or from a production environment, etc., when the NiCrFe alloy is industrially produced, and which is permitted within a range not adversely affecting the NiCrFe alloy of the present embodiment.
  • NiCrFe alloy according to the present invention may contain B in place of part of Fe.
  • B Boron
  • B is an optional element and may not be contained.
  • B increases the creep strength of the alloy by causing grain boundary carbides to be finely dispersed. Further, B segregates in grain boundaries to assist the effects of REM.
  • the B content is 0 to 0.010%.
  • the upper limit of the B content is preferably 0.008%.
  • the lower limit of the B content to effectively obtain the aforementioned effects is preferably 0.0001%, and more preferably 0.0005%.
  • NiCrFe alloy according to the present invention may contain one or two types selected from the group consisting of Ca and Mg in place of part of Fe. Each of these elements forms a compound with S, thereby assisting the effects of REM.
  • Calcium (Ca) is an optional element and may not be contained. When contained, Ca forms a compound with S, thereby assisting the S immobilizing effect of REM. If Ca is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the Ca content is too high, Ca forms oxide, and deteriorates the hot workability of the alloy. Therefore, the Ca content is 0 to 0.010%.
  • the upper limit of the Ca content is preferably 0.008%.
  • the lower limit of the Ca content to effectively obtain the aforementioned effect is preferably 0.0001%, more preferably 0.0002% and further preferably 0.0003%.
  • Magnesium (Mg) is an optional element and may not be contained. When contained, Mg forms a compound with S, thereby assisting the S immobilizing effect of REM. When Mg is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the Mg content is too high, Mg forms oxide, thereby deteriorating the hot workability of the alloy. Therefore, the Mg content is 0 to 0.010%.
  • the upper limit of the Mg content is preferably 0.008%.
  • the lower limit of the Mg content to effectively obtain the aforementioned effect is preferably 0.0001%, more preferably 0.0002% and further preferably 0.0003%.
  • NiCrFe alloy according to the present invention may contain one or more types selected from the group consisting of V, Nb, Ta, and Hf in place of part of Fe. Each of these elements forms carbide and carbonitride, thereby increasing the creep strength of the alloy.
  • Vanadium (V) is an optional element and may not be contained. When contained, V forms fine carbide and carbonitride with C and N, thereby increasing the creep strength of the alloy. When V is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the V content is too high, a large amount of carbide and carbonitride will precipitate, thereby deteriorating the creep ductility of the alloy. Therefore, the V content is 0 to 0.5%. The upper limit of the V content is preferably 0.4%. The lower limit of the V content to effectively obtain the aforementioned effect is 0.01%.
  • Niobium (Nb) is an optional element and may not be contained. When contained, Nb forms fine carbide and carbonitride with C and N, thereby increasing the creep strength of the alloy. When Nb is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the Nb content is too high, a large amount of carbide and carbonitride will precipitate, thereby deteriorating the creep ductility and toughness of the alloy. Therefore, the Nb content is 0 to 1.0%. The upper limit of the Nb content is preferably 0.4%. The lower limit of the Nb content to effectively obtain the aforementioned effect is 0.01%.
  • Tantalum (Ta) is an optional element and may not be contained. When contained, Ta forms fine carbide and carbonitride with C and N, thereby increasing the creep strength of the alloy. When Ta is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the Ta content is too high, a large amount of carbide and carbonitride will precipitate, thereby deteriorating the creep ductility and toughness of the alloy. Therefore, the Ta content is 0 to 1.0%. The upper limit of the Ta content is preferably 0.4%. The lower limit of the Ta content to effectively obtain the aforementioned effect is 0.01%.
  • Hafnium (Hf) is an optional element and may not be contained. When contained, Hf forms fine carbide and carbonitride with C and N, thereby increasing the creep strength of the alloy. When Hf is contained in any small amount, the aforementioned effect will be obtained to some degree. However, when the Hf content is too high, a large amount of carbide and carbonitride will precipitate, thereby deteriorating the creep ductility and toughness of the alloy. Therefore, the Hf content is 0 to 1.0%. The upper limit of the Hf content is preferably 0.4%. The lower limit of the Hf content to effectively obtain the aforementioned effect is 0.01%.
  • NiCrFe alloy according to the present invention may contain one or more types selected from the group consisting of Mo, W, Co, and Cu in place of part of Fe.
  • Molybdenum (Mo) is an optional element and may not be contained. When contained, Mo dissolves into the alloy, thereby increasing the creep strength of the alloy at high temperatures. When Mo is contained in any small amount, such effect will be obtained to some degree. However, when the Mo content is too high, the stability of austenite will be lost, thereby deteriorating the toughness of the alloy. Therefore, the Mo content is 0 to 1.0%. The upper limit of the Mo content is preferably 0.9%. The lower limit to effectively obtain the aforementioned effect is preferably 0.01%.
  • Tungsten (W) is an optional element and may not be contained. When contained, W dissolves into the alloy, thereby increasing the creep strength of the alloy at high temperatures. When W is contained in any small amount, such effect will be obtained to some degree. However, when the W content is too high, the stability of austenite will be lost, thereby deteriorating the toughness of the alloy. Therefore, the W content is 0 to 2.0%. The upper limit of the W content is preferably 1.8%. The lower limit of the W content to effectively obtain the aforementioned effect is preferably 0.01%.
  • Co Co
  • Co is an optional element and may not be contained. When contained, Co stabilizes austenite and dissolves into the alloy, thereby increasing the creep strength of the alloy at high temperatures. When Co is contained in any small amount, such effects will be obtained to some degree. However, when the Co content is too high, the production cost increases. Therefore, the Co content is 0 to 3.0%.
  • the upper limit of the Co content is preferably 2.8%.
  • the lower limit of the Co content to effectively obtain the aforementioned effects is preferably 0.01%.
  • Cupper (Cu) is an optional element and may not be contained.
  • Cu stabilizes austenite and suppresses precipitation of brittle phase such as ⁇ phase during use at high temperatures.
  • the Cu content is 0 to 3.0%.
  • the upper limit of the Cu content is preferably 2.5%, and more preferably less than 2.0%.
  • the lower limit of the Cu content to effectively obtain the aforementioned effects is preferably 0.01%.
  • NiCrFe alloy according to the present invention further satisfies Formula (1): 0.50 ⁇ Ti + 48 Al / 27 ⁇ 2.20 where, each symbol of element in Formula (1) is substituted by the content (mass%) of the corresponding element.
  • fn1 Ti + 48A1/27 is an index to indicate the precipitation amount of ⁇ '.
  • fn1 indicates a total amount of Ti when the amount of Al is converted into the amount of Ti.
  • fn1 is less than 0.50, a sufficient precipitation amount of ⁇ ' will not be obtained, so that the NiCrFe alloy cannot obtain excellent creep resistance.
  • fn1 is more than 2.20, the stress relaxation cracking resistance, creep ductility, and toughness of the alloy will deteriorate due to an excessive precipitation amount of ⁇ '. Therefore, fn1 is 0.50 to 2.20. In this range, an appropriate amount of ⁇ ' is precipitated, and excellent creep resistance is obtained.
  • the upper limit of the fn1 is preferably 2.00.
  • the lower limit of fn1 is preferably 0.65.
  • the above described chemical composition further satisfies Formula (2): 0.40 ⁇ Ti / Ti + 48 Al / 27 ⁇ 0.80 where, each symbol of element in Formula (2) is substituted by the content (mass%) of the corresponding element.
  • fn2 Ti/(Ti + 48A1/27) is a ratio of the Ti content with respect to the total content of Al and Ti, the content of Al being converted into the amount of Ti.
  • fn2 is less than 0.40, the Ti content is too low with respect to the Al content, and the precipitation amount of ⁇ ' decreases. As a result, the NiCrFe alloy cannot obtain excellent creep strength.
  • fn2 is more than 0.80, the Ti content becomes excessive with respect to the Al content so that although fine ⁇ ' precipitates in an early stage of creep, the ⁇ ' changes to coarse and acicular ⁇ phase over time. As a result, the creep strength and toughness of the alloy deteriorate. Therefore, fn2 is 0.40 to 0.80. In this range, ⁇ ' precipitates in an appropriate amount, and will not change to ⁇ phase even when further time passes so that excellent creep strength is obtained.
  • the upper limit of fn2 is preferably 0.75.
  • the above described chemical composition further satisfies Formula (3): ⁇ REM / A REM ⁇ S / 32 ⁇ 2 / 3 ⁇ O / 16 ⁇ 0 where, each symbol of element in Formula (3) is substituted by the content (mass%) of the corresponding element, and A(REM) is substituted by the atomic weight of each REM.
  • fn3 ⁇ [REM/(A(REM))] - S/32 - 2/3•O/16 is an index to indicate the amount of S that segregates in grain boundaries.
  • fn3 is a negative value, S segregates in grain boundaries, thereby resulting in grain boundary embrittlement so that the stress relaxation cracking resistance of the alloy deteriorates.
  • fn3 is not less than 0, REM immobilizes S as inclusions, thereby decreasing the S content in the matrix. As a result, it is possible to improve the stress relaxation cracking resistance of the alloy. Therefore, fn3 is not less than 0.
  • the production method of the present embodiment comprises a process of producing an ingot (steelmaking process), and a process of producing a hot-rolled plate (hot working process).
  • a process of producing an ingot steelmaking process
  • a process of producing a hot-rolled plate hot working process
  • alloys having the above described chemical compositions are melted.
  • the melting is performed by using, for example, the high-frequency induction vacuum melting.
  • an ingot is produced by an ingot-making method.
  • hot working is performed once or multiple times.
  • the ingot is heated, and thereafter hot working is performed.
  • the hot working refers to, for example, hot forging and hot rolling.
  • the hot working may be performed by a well-known method.
  • the hot-worked NiCrFe alloy may be subjected to cold working.
  • the cold working is, for example, cold rolling.
  • the NiCrFe alloy which has been subjected to the above described working, may be subjected to heat treatment.
  • the heat treatment temperature is preferably 1050 to 1200°C.
  • the NiCrFe alloy is preferably water cooled.
  • the NiCrFe alloy may be a bar or an alloy pipe.
  • the shape of the product will not be limited.
  • it is preferable that hot working by hot extrusion is performed.
  • NiCrFe alloy produced by the processes described so far has excellent creep strength and excellent stress relaxation cracking resistance.
  • ⁇ ' and ⁇ phase precipitate in a use environment at high temperatures.
  • the microstructure of the NiCrFe alloy according to the present invention after being kept at 650°C for 3000 hours contains a total of 2 to 6 mass% of ⁇ ' and ⁇ phase, wherein the number density of ⁇ phase is less than 5/100 ⁇ m 2 .
  • the ⁇ ' and ⁇ phase are herein also collectively referred to as "aging precipitates”.
  • the precipitation amount of ⁇ ' in the alloy will be decreased.
  • the NiCrFe alloy cannot obtain excellent creep strength.
  • the precipitation amount of ⁇ ' may excessively increase. In that case, the alloy cannot obtain excellent stress relaxation cracking resistance. Therefore, the total of ⁇ ' and ⁇ phase after aging treatment is 2 to 6 mass%.
  • the total of ⁇ ' and ⁇ phase can be measured by the following method.
  • the NiCrFe alloy according to the present invention is subjected to aging treatment for keeping the alloy at 650°C for 3000 hours.
  • a test specimen of 10 mm ⁇ 5 mm ⁇ 50 mm is sampled from the NiCrFe alloy after the aging treatment.
  • the alloy is an alloy plate
  • the test specimen is sampled from a middle part of plate thickness of the alloy pipe.
  • the test specimen is sampled from a middle part of wall thickness. Note that the weight of the test specimen is measured in advance.
  • the sampled test specimen is electrolyzed in a 1% tartaric acid-1% (NH 4 ) 2 SO 4 -water solution to sample the residue from the electrolyte.
  • the sampled residue is melted by HCl (1+4)-20% tartaric acid solution of 60°C and the solution is filtered.
  • the filtrate is measured by ICP emission spectrometry to determine Ti, Al, and Ni concentrations in the residue. From the determined Ti, Al, and Ni concentrations in the residue, and the weight of the test specimen, Ti, Al, and Ni contents in the ⁇ ' and ⁇ phase of the test specimen are determined.
  • the sum of Ti, Al, and Ni contents which have been determined by the method described so far, is defined as a sum of ⁇ ' and ⁇ phase (mass%).
  • the NiCrFe alloy according to the present invention is subjected to aging treatment for keeping the alloy at 650°C for 3000 hours and then the number density of ⁇ phase is not less than 5/100 ⁇ m 2 , part of ⁇ ' has changed to ⁇ phase. For that reason, the NiCrFe alloy cannot obtain excellent creep strength. Therefore, the number density of ⁇ phase after aging treatment is less than 5/100 ⁇ m 2 .
  • the number density of ⁇ phase can be measured by the following method.
  • the NiCrFe alloy according to the present invention is subjected to aging treatment for keeping the alloy at 650°C for 3000 hours.
  • Microscopic observation is performed on the NiCrFe alloy after aging treatment.
  • a microscopic test specimen is sampled from the NiCrFe alloy after aging treatment.
  • the alloy is an alloy plate
  • the test specimen is sampled from a middle part of the plate thickness.
  • the alloy is an alloy pipe
  • the microscopic test specimen is sampled from a middle part of wall thickness of the alloy pipe.
  • the sampled microscopic test specimen is subjected to mechanical polishing.
  • the surface of the microscopic test specimen after mechanical polishing is electrolytically corroded by 10% oxalic acid.
  • the microscopic test specimen after electrolytic corrosion is observed by a scanning electron microscope (SEM) in 5 visual fields, and an SEM image is created for each visual field.
  • the observation magnification is 10000 times, and observation field is, for example, 12 ⁇ m ⁇ 9 ⁇ m.
  • the ⁇ ' and ⁇ phase differ in their shapes. Specifically, ⁇ ' is observed to be spherical and ⁇ phase be acicular. More specifically, an aspect ratio of ⁇ ' is less than 3, and an aspect ratio of ⁇ phase is not less than 3.
  • the term "aspect ratio" means a value obtained by dividing the major axis length by the minor axis length for each aging precipitate.
  • aging precipitates ( ⁇ ' and ⁇ phase) are identified from contrast. Further, by image processing, aspect ratios are calculated for the identified aging precipitates. To calculate an aspect ratios, general purpose application software may be used. When a calculated aspect ratio is not less than 3, the aging precipitate is identified to be ⁇ phase.
  • the number of identified ⁇ phase is counted to determine a sum of the numbers in all visual fields.
  • the number density of ⁇ phase in an observation field of 100 ⁇ m 2 (number/100 ⁇ m 2 ) is determined.
  • NiCrFe alloy plate materials were produced. Using thus produced NiCrFe alloy plate materials, the following tests were conducted.
  • a test specimen was fabricated from the produced alloy plate material.
  • the test specimen was sampled from a central part of thickness of the alloy plate material in parallel with the longitudinal direction (rolling direction).
  • the specimen was a round bar test specimen, whose parallel part had a diameter of 6 mm, and which had a gauge length of 30 mm.
  • the creep rupture test was conducted. The creep rupture test was performed under a tensile load of 70 MPa in the air atmosphere of 750°C.
  • a test specimen whose rupture time was not less than 3000 hours was evaluated as "E" (Excellent), and those whose rupture time was less than 3000 hours as "NA" (Not Acceptable).
  • test specimens were fabricated by the above described method.
  • the fabricated test specimens were subjected to aging treatment to keep them at 650°C for 3000 hours, and the sum (mass%) of ⁇ ' and ⁇ phase of each test specimen was determined by the above described method. Further, the number density of ⁇ phase (number/100 ⁇ m 2 ) was determined by the above described method.
  • a sum of ⁇ ' and ⁇ phase of less than 2 mass% was evaluated as "L" (Less), that of 2 to 6 mass% as "E” (Excellent), and that of more than 6 mass% as "TM” (Too Much). Further, those showed a number density of ⁇ phase of not less than 5/100 ⁇ m 2 were evaluated as " ⁇ ".
  • the produced alloy plate material was further subjected to cold working. Specifically, cold rolling was performed on the alloy plate material until its thickness became 12 mm. The reduction of area of this cold rolling was 20%.
  • a test specimen was fabricated from this alloy plate material. The test specimen was sampled from a central part of thickness of the alloy plate material in parallel with the longitudinal direction (rolling direction). The specimen was a round bar test specimen, whose parallel part had a diameter of 6 mm, and which had a gauge length of 30 mm. By using the specimen, a stress relaxation cracking test was conducted. The stress relaxation cracking test was conducted such that the test specimen is subjected to tensile strain 10% at a strain rate of 0.05 min -1 and is kept as is for 300 hours in air atmosphere of 650°C. A specimen which did not rupture after being kept for 300 hours was evaluated as "E" (Excellent), and one which ruptured as "NA” (Not Acceptable).
  • the present invention can be widely applied to uses for which high creep strength and stress relaxation cracking resistance are demanded.
  • the present invention can be suitably used for high temperature members of thermal power generation boilers, petroleum refining and chemical industry plants, or the like.

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Claims (6)

  1. Alliage NiCrFe, comprenant une composition chimique constitué par : en % en masse,
    C: 0,03 à 0,15%,
    Si: pas plus de 1,00%,
    Mn: pas plus de 2,00%,
    P: pas plus de 0,040%,
    S: pas plus de 0,0050%,
    Cr: 18,0 à 25,0%,
    Ni: 25,0 à 40,0%,
    Ti: 0,10 à 1,60%,
    Al: 0,05 à 1,00%,
    N: pas plus de 0,020%,
    O: pas plus de 0,008%,
    Terres rares (REM): 0,001 à 0,100%,
    B: 0 à 0,010%,
    Ca: 0 à 0,010%,
    Mg: 0 à 0,010%,
    V: 0 à 0,5%,
    Nb: 0 à 1,0%,
    Ta: 0 à 1,0%,
    Hf: 0 à 1,0%,
    Mo: 0 à 1,0%,
    W: 0 à 2,0%,
    Co: 0 à 3,0%
    et Cu: 0 à 3,0%, le reste étant du Fe et des impuretés, la composition chimique satisfaisant aux formules (1) à (3) suivantes: 0.50 ≤ Ti + 48 Al / 27 ≤ 2.20
    Figure imgb0019
     0.40 ≤ Ti / Ti + 48 Al / 27 ≤ 0.80
    Figure imgb0020
     ∑ REM / A REM − S / 32 − 2 / 3 · O / 16 ≥ 0
    Figure imgb0021
     où, chaque symbole d'élément des formules (1) à (3) est remplacé par la teneur en % en masse de l'élément correspondant, et A(REM) dans la formule (3) est remplacé par le poids atomique de chaque terre rare.
  2. Alliage NiCrFe selon la revendication 1, dans lequel
    la composition chimique contient
    B: 0,0001 à 0,010%.
  3. Alliage NiCrFe selon la revendication 1 ou 2, dans lequel
    la composition chimique contient un ou deux types choisis dans le groupe constitué par
    Ca: 0,0001 à 0,010%, et
    Mg: 0,0001 à 0,010.
  4. Alliage NiCrFe selon l'une quelconque des revendications 1 à 3, dans lequel la composition chimique contient un ou plusieurs types choisis dans le groupe constitué par
    V: 0,01 à 0,5%,
    Nb: 0,01 à 1,0%,
    Ta: 0,01 à 1,0%, et
    Hf: 0,01 à 1,0%.
  5. Alliage NiCrFe selon l'une quelconque des revendications 1 à 4, dans lequel la composition chimique contient un ou plusieurs types choisis dans le groupe constitué par
    Mo: 0,01 à 1,0%,
    W: 0,01 à 2,0%,
    Co: 0,01 à 3,0%, et
    Cu: 0,01 à 3,0%.
  6. Alliage NiCrFe selon l'une quelconque des revendications 1 à 5, dans lequel l'alliage NiCrFe ne se rompt pas pendant 300 heures ou plus dans un essai de relaxation des contraintes dans lequel l'alliage NiCrFe est soumis à une déformation en traction de 10% à un taux de déformation de 0,05 min-1 et maintenu tel quel dans une atmosphère d'air de 650 °C après avoir été soumis à un laminage à froid à une réduction de surface de 20%.
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