WO2012026344A1 - 含Crオーステナイト合金管およびその製造方法 - Google Patents
含Crオーステナイト合金管およびその製造方法 Download PDFInfo
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- WO2012026344A1 WO2012026344A1 PCT/JP2011/068414 JP2011068414W WO2012026344A1 WO 2012026344 A1 WO2012026344 A1 WO 2012026344A1 JP 2011068414 W JP2011068414 W JP 2011068414W WO 2012026344 A1 WO2012026344 A1 WO 2012026344A1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
- C23C8/18—Oxidising of ferrous surfaces
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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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
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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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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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
- C22C38/18—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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L9/00—Rigid pipes
- F16L9/02—Rigid pipes of metal
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21D—NUCLEAR POWER PLANT
- G21D1/00—Details of nuclear power plant
- G21D1/006—Details of nuclear power plant primary side of steam generators
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Definitions
- the present invention relates to a Cr-containing austenitic alloy tube with little Ni elution even when used for a long period of time in a high-temperature water environment, and a method for producing the same, and in particular, a Cr-containing austenitic alloy tube suitable for applications such as nuclear plant components And a manufacturing method thereof.
- ⁇ Cr-containing austenitic alloy pipes are used as various members because of their excellent mechanical properties.
- Cr-containing austenitic alloy tubes having excellent corrosion resistance are used.
- 60% Ni-30% Cr-10% Fe alloy or the like is used for a steam generator member of a pressurized water reactor (PWR).
- Cr-containing austenitic alloy tubes used as heat transfer tubes for steam generators for nuclear power plants contain a large amount of Ni and are excellent in corrosion resistance and have a low corrosion rate. However, trace amounts of Ni are eluted from the base material after long-term use.
- Ni is transported to the core in the process of circulating the reactor water and irradiated with neutrons in the vicinity of the fuel.
- Ni is irradiated with neutron, it is converted to radioactive Co by nuclear reaction. Since this radioactive Co has a very long half-life, it continues to emit radiation for a long time. Therefore, if the amount of Ni elution increases, the periodic inspection cannot be started until the radiation dose released has decreased to an appropriate value, so that the period of the periodic inspection is extended and an economic loss is incurred.
- Patent Document 1 a Ni-based alloy heat transfer tube is annealed in a temperature range of 400 to 750 ° C. in an atmosphere with a vacuum degree of 10 ⁇ 2 to 10 ⁇ 4 Torr to form an oxide film mainly composed of chromium oxide. And a method for improving the general corrosion resistance is disclosed.
- Patent Document 2 discloses a heat treatment that combines at least a part of an age hardening treatment and an oxide film forming treatment in an oxidizing atmosphere of 10 ⁇ 3 Torr to atmospheric pressure after solution treatment of a Ni-based precipitation strengthened alloy. The manufacturing method of the member for nuclear power plants which gives is disclosed.
- Patent Document 3 discloses a method for producing a Ni-based alloy product in which a Ni-based alloy product is heat-treated in a mixed atmosphere of hydrogen or hydrogen and argon having a dew point of ⁇ 60 ° C. to + 20 ° C.
- Patent Document 4 discloses a method of forming a chromium-enriched layer by exposing an alloy workpiece containing Ni and Cr to a gas mixture of water vapor and at least one non-oxidizing gas.
- Patent Document 5 discloses a continuous heat treatment furnace as a heat treatment method that reliably and efficiently produces an oxide film having a two-layer structure that suppresses elution of Ni in a high-temperature water environment on the inner surface of a Ni-based alloy tube. At least two gas supply devices are provided on the side, or one gas supply device is provided on each of the outlet side and the inlet side, and one of these gas supply devices and a gas introduction pipe penetrating through the furnace are provided.
- the atmosphere of the work tube before charging into the heat treatment furnace consisting of hydrogen or a mixture of hydrogen and argon with a dew point in the range of -60 ° C to + 20 ° C from the front end in the direction of travel
- supplying the tube to the furnace while supplying gas and holding it at 650 to 1200 ° C for 1 to 1200 minutes after the tip of the tube reaches the exit side of the furnace, supply atmospheric gas to the inside of the tube
- a heat treatment method that repeats an operation of switching to supply from a gas supply device is disclosed. That.
- Ni-based alloy is made of a heat treatment atmosphere made of carbon dioxide gas, or at least 0.0001 Vol.% Carbon dioxide gas, 99.9999 Vol.% Hydrogen gas, and 99.9999 Vol.% Rare gas.
- a manufacturing method is disclosed in which an oxide film made of chromium oxide is formed on the surface of a Ni-based alloy by treatment in an atmosphere consisting of one kind.
- Patent Documents 7 and 8 disclose a manufacturing method for forming a chromium oxide film having a predetermined thickness on the inner surface of a tube by treating a Cr-containing nickel-based alloy tube in an atmosphere made of a non-oxidizing gas containing carbon dioxide. Is disclosed.
- Patent Document 1 Since the film formed by the method disclosed in Patent Document 1 has an insufficient thickness, there is a problem that the elution prevention effect is lost when the film is damaged by long-term use.
- the method disclosed in Patent Document 2 has a problem that oxidized Ni is easily taken into the film and this Ni is eluted during use.
- As the oxidizing gas that oxidizes the tube water vapor, oxygen, and the like can be considered, but water vapor is considered most suitable from the viewpoint of safety and cost.
- the coating provided on the pipe is required to have a sufficiently thick film thickness to exhibit corrosion resistance and uniformity in the pipe length and pipe circumferential direction of the coating thickness from the viewpoint of quality.
- Patent Documents 3 to 5 for controlling the water vapor amount (dew point) to form an oxide film cannot satisfy these requirements. This is because, at the inlet to which a high-concentration raw material is supplied, the reaction rate becomes faster and the film becomes thicker, and the closer to the outlet, the more the raw material is consumed and the concentration decreases, and the outlet film becomes thinner.
- steam is highly reactive, and oxidation of Ni-based alloy tubes requires high temperatures (1000-1200 ° C), so there is a large difference in the amount of reaction between the inlet and outlet, and a uniform oxide film is formed throughout the entire tube. It is difficult to form. If the thickness of the oxide film is too thin, the effect of Ni elution resistance cannot be obtained.
- the thickness is too thick, the oxide film easily peels off, and conversely, the Ni elution resistance deteriorates. According to the study by the present inventors, it is necessary to adjust the thickness of the oxide film in the order of micron order to submicron order.
- Patent Documents 6 to 8 adopt gas conditions using carbon dioxide, which is less reactive than water vapor, as the oxidizing gas, and aim to improve the uniformity of the film.
- carbon dioxide generates harmful carbon monoxide after metal oxidation.
- the Ni-based alloy may be carburized by the generated carbon monoxide, so it cannot be said to be a method for providing a safe and high-quality product.
- the present inventors have conducted intensive research and limited the gas conditions centered on the flow rate, as well as the length of the tube to be treated and the diameter of the tube, by using safe and inexpensive water vapor as the oxidizing gas. Thus, the present inventors have found that it is possible to control the thickness of the long Cr-containing austenitic alloy pipe film even when highly reactive water vapor is used.
- An object of the present invention is to provide a method for producing a Cr-containing austenitic alloy tube and a Cr-containing austenitic alloy tube in which chromium oxide is uniformly formed on the surface of the Cr-containing austenitic alloy tube at a low cost.
- the gist of the present invention is a method for producing Cr-containing austenitic alloy tubes shown in the following (1) to (4) and Cr-containing austenitic alloy tubes shown in (5) to (10) below.
- ⁇ 1 and ⁇ 2 are the thicknesses ( ⁇ m) of the chromium oxide films at both ends of the tube.
- a non-oxidizing gas containing water vapor is circulated and heated on the inner surface of the Cr-containing austenitic alloy tube, and the inner surface of the Cr-containing austenitic alloy tube has a thickness of 0.05 to 1.5 ⁇ m and the following (i A method for producing a Cr-containing austenitic alloy tube, characterized by forming a chromium oxide film satisfying the relationship defined by the formula (1). 0.4 ⁇ ⁇ 1 / ⁇ 2 ⁇ 2.5 (i)
- ⁇ 1 and ⁇ 2 are the thicknesses ( ⁇ m) of the chromium oxide films at both ends of the tube.
- Heating is carried out under the condition that the non-oxidizing gas containing 250 to 25000 ppm of water vapor is circulated in the pipe at a rate of 6.0 to 50 L / min and maintained at a temperature range of 800 to 1200 ° C. for 1 minute or longer.
- the method for producing a Cr-containing austenitic alloy pipe according to the above (5) is carried out under the condition that the non-oxidizing gas containing 250 to 25000 ppm of water vapor is circulated in the pipe at a rate of 6.0 to 50 L / min and maintained at a temperature range of 800 to 1200 ° C. for 1 minute or longer.
- the "chromium oxide film” means an oxide film mainly composed of Cr 2 O 3, oxides other than Cr 2 O 3, for example, MnCr 2 O 4, TiO 2 , Al 2 O 3, An oxide such as SiO 2 may be included. Further, if the surface of the Cr-containing austenitic alloy tube has an oxide film made of chromium oxide, another oxide layer is formed on the upper layer (outer layer) and / or lower layer (inner layer) of the chromium oxide layer. May be formed.
- a chromium oxide film can be uniformly and inexpensively formed on the inner surface of a Cr-containing austenitic alloy tube.
- the Cr-containing austenitic alloy tube manufactured by the method of the present invention has a very low elution of Ni even when used for a long time in a high-temperature water environment, for example, a high-temperature water environment in a nuclear power plant. It is most suitable for members used in high-temperature water such as generator (tubing), especially for nuclear power plants.
- the Ni elution resistance depends on the thickness of the chromium oxide film, it is necessary to control the film thickness. When the film thickness is less than 0.05 ⁇ m, the Ni elution resistance is insufficient. A film thickness of 0.05 ⁇ m or more exhibits sufficient corrosion resistance, but is preferably 0.1 ⁇ m or more. On the other hand, in a high Ni alloy in which the Ni content exceeds 40%, the film thickness is more preferably 0.2 ⁇ m or more, and further preferably 0.3 ⁇ m or more.
- the thickness of the film is 1.5 ⁇ m or less.
- the upper limit of the film thickness is desirably 0.95 ⁇ m, and the more desirable upper limit is 0.85 ⁇ m.
- the thickness of the chromium oxide film satisfies the relationship defined by the following formula (i). 0.4 ⁇ ⁇ 1 / ⁇ 2 ⁇ 2.5 (i)
- ⁇ 1 and ⁇ 2 are the thicknesses ( ⁇ m) of the chromium oxide films at both ends of the tube.
- the above formula (i) is 0.5 ⁇ ⁇ 1 / ⁇ 2 ⁇ 2.0 Is preferable, 0.70 ⁇ ⁇ 1 / ⁇ 2 ⁇ 1.55 Is more preferable.
- the Cr-containing austenitic alloy tube is heated on the inner surface of the Cr-containing austenitic alloy tube by heating with an atmospheric gas composed of water vapor and a non-oxidizing gas. A chromium oxide film is formed.
- the supply of the oxidizing gas is considered to limit the oxidation reaction.
- an atmospheric gas is supplied into the pipe, a concentration gradient is generated.
- the gas diffusivity at this time is considered to depend on the oxidizing gas concentration and the flow rate of the atmospheric gas. Since the supply of the oxidizing gas depends on the gas diffusibility, it can be considered that it also depends on the oxidizing gas concentration and the flow rate of the atmospheric gas.
- C average concentration within the range of 5-10 ⁇ m depth from the surface layer on the inner surface side of the tube is the concentration within the range of 5-10 ⁇ m in the general depth analysis (GDS, XPS, SIMS) at 0.1 ⁇ m pitch or less. It is a value calculated and averaged.
- GDS, XPS, SIMS general depth analysis
- an analysis value obtained by a high-frequency combustion infrared absorption method using a cutting sample collected from the central portion of the tube thickness was used.
- an atmospheric gas containing water vapor as the atmospheric gas supplied into the tube, and further clean (for example, degrease) the inside of the tube.
- an oxide film having a uniform film thickness can be formed by adjusting the water vapor concentration in the atmospheric gas and the flow rate of the atmospheric gas within an appropriate range.
- the upper limit of the water vapor concentration is not particularly limited, but is preferably 25000 ppm or less from the viewpoint of reducing the production cost.
- oxygen may be partially supplied in addition to water vapor as the oxidizing gas.
- Oxygen can form chromium oxide as well as water vapor.
- the content of oxygen gas is preferably 10,000 ppm or less. This is because when a large amount of oxygen gas is contained, the formation of a chromium oxide film is promoted, the Cr concentration in the base material is lowered, and the corrosion resistance is deteriorated. If oxygen is contained even in a very small amount, the above effect is exhibited, so the lower limit is not particularly set. However, the effect becomes remarkable when 0.0001 vol% or more is contained.
- non-oxidizing gas examples include hydrogen gas, rare gas (Ar, He, etc.), carbon monoxide gas, nitrogen gas, hydrocarbon gas, and the like.
- these non-oxidizing gases when carbon monoxide gas, nitrogen gas, or hydrocarbon gas is used, there is a concern of carburizing or nitriding, and therefore it is preferable that at least one of hydrogen gas and rare gas is included. .
- hydrogen gas is often used industrially as an atmosphere gas for heat treatment, and if it is used for dilution of water vapor gas, the manufacturing cost can be reduced. Therefore, it is most preferable to perform the heat treatment with the atmosphere gas as a gas atmosphere composed of water vapor gas and hydrogen gas.
- oxygen may be supplied as an oxidizing gas to react hydrogen and oxygen to produce water, which may be used for oxidation of the tube. In that case, be careful of explosion.
- the concentration of atmospheric gas in the case of containing water vapor can be controlled by adjusting the water vapor concentration by dew point management after adjusting the concentration of water vapor gas and non-oxidizing gas or oxygen gas. Further, after adjusting the dew point using a non-oxidizing gas, water vapor gas or further oxygen gas may be added.
- the flow rate of the atmospheric gas supplied to the inner surface of the tube is preferably 6.0 to 50 L / min. If it is less than 6.0 L / min, an oxide film with a desired thickness cannot be formed even if the water vapor concentration and heating conditions are adjusted. On the other hand, when it exceeds 50 L / min, the oxide film becomes excessively thick.
- Tube length and inner diameter Cr-containing austenitic alloy tubes manufactured under the water vapor concentration and heat treatment conditions specified in the present invention are steam for nuclear power plants having a tube length of 5 to 50 m and a tube inner diameter of 10 to 30 mm. Suitable for heat transfer tubes for generators.
- the coating thickness variation tends to increase.
- the oxide film thickness on the inner surface of the tube can be adjusted by appropriately adjusting the concentration of water vapor and the gas flow rate according to the length and inner diameter of the tube. The variation of the can be reduced.
- the heating temperature may be in a range where an appropriate oxide film thickness and composition and strength characteristics of the alloy can be obtained. Specifically, when the heating temperature is less than 800 ° C., chromium may be insufficiently oxidized. In order to obtain a film having an appropriate film thickness in an appropriate time, 900 ° C. or higher is preferable. More preferably, it is 1000 ° C. or higher. On the other hand, the upper limit is 1200 ° C. If it exceeds 1200 ° C, the strength of the Cr-containing austenitic alloy tube may not be secured. Therefore, the heating temperature is preferably in the range of 800 to 1200 ° C.
- the heating time may be set within a range in which an appropriate oxide film thickness and composition can be obtained. That is, it is desirable to heat for 1 minute or longer in order to form an oxide film mainly composed of chromium oxide.
- the upper limit is not particularly defined, but at least in the temperature range of 800 to 1200 ° C. preferred in the present invention, even when heated for more than 24 hours, an oxide film is hardly formed, which is disadvantageous from the viewpoint of production cost. Therefore, the heating time is preferably in the range of 1 minute to 24 hours.
- the chemical composition of the raw tube of the Cr-containing austenitic alloy tube used in the production method of the present invention is, for example, mass%, C: 0.15% or less, Si: 1.00 %: Mn: 2.0% or less, P: 0.030% or less, S: 0.030% or less, Cr: 10.0-40.0%, Ni: 8.0-80.0%, Ti: 0.5% or less, Cu: 0.6% or less, Al: 0.5 % Or less and N: 0.20% or less, with the balance being Fe and impurities.
- impurities are components mixed in due to various factors of raw materials such as ores and scraps and manufacturing processes when the alloy is industrially manufactured, and are allowed within a range that does not adversely affect the present invention. Means something.
- C 0.15% or less If C exceeds 0.15%, the stress corrosion cracking resistance may deteriorate. Therefore, when C is contained, the content is desirably 0.15% or less. More desirable is 0.06% or less. C has the effect of increasing the grain boundary strength of the alloy. In order to obtain this effect, the C content is desirably 0.01% or more.
- Si 1.00% or less Si is used as a deoxidizer during smelting and remains as an impurity in the alloy. At this time, it should be limited to 1.00% or less. If the content exceeds 0.50%, the cleanliness of the alloy may decrease, so it is more desirable to limit the Si content to 0.50% or less.
- Mn 2.0% or less If Mn exceeds 2.0%, the corrosion resistance of the alloy is lowered. More desirable is 1.0% or less. Mn has a lower free energy of formation of oxide than Cr and precipitates as MnCr 2 O 4 by heating. Further, since the diffusion rate is relatively fast, usually, Cr 2 O 3 is preferentially generated in the vicinity of the base material by heating, and MnCr 2 O 4 is formed as an upper layer outside thereof. If the MnCr 2 O 4 layer is present, the Cr 2 O 3 layer is protected in the use environment, and even if the Cr 2 O 3 layer is destroyed for some reason, the MnCr 2 O 4 repairs the Cr 2 O 3 Is promoted. Such an effect becomes remarkable when the content is 0.1% or more.
- P 0.030% or less
- P is an element present as an impurity in the alloy. If its content exceeds 0.030%, corrosion resistance may be adversely affected. Therefore, it is desirable to limit the P content to 0.030% or less.
- S 0.030% or less S is an element present as an impurity in the alloy. If its content exceeds 0.030%, corrosion resistance may be adversely affected. Therefore, it is desirable to limit the S content to 0.030% or less.
- Cr 10.0-40.0% Cr is an element necessary for producing an oxide film made of chromium oxide. In order to form such an oxide film on the alloy surface, it is desirable to contain 10.0% or more. However, if it exceeds 40.0%, workability may deteriorate. Accordingly, the Cr content is desirably 10.0 to 40.0%.
- Ni 8.0-80.0%
- Ni is an element necessary for ensuring the corrosion resistance of the Cr-containing austenitic alloy, and it is desirable to contain 8.0% or more.
- Ni since Ni is expensive, it may be contained as much as necessary depending on the application, and is preferably 80.0% or less.
- Ti 0.5% or less Ti has a risk of degrading the cleanliness of the alloy if its content exceeds 0.5%. Therefore, its content is preferably 0.5% or less. More desirable is 0.4% or less. However, from the viewpoint of improving the workability of the alloy and suppressing grain growth during welding, it is desirable to contain 0.1% or more.
- Cu 0.6% or less
- Cu is an element present as an impurity in the alloy. If the content exceeds 0.6%, the corrosion resistance of the alloy may be lowered. Therefore, it is desirable to limit the Cu content to 0.6% or less.
- Al 0.5% or less Al is used as a deoxidizer during steelmaking and remains as an impurity in the alloy. The remaining Al becomes oxide inclusions in the alloy, which deteriorates the cleanliness of the alloy and may adversely affect the corrosion resistance and mechanical properties of the alloy. Therefore, it is desirable to limit the Al content to 0.5% or less.
- N 0.20% or less N may not be added, but the Cr-containing austenitic alloy targeted by the present invention usually contains about 0.01% of N as an impurity. However, if N is positively added, the strength can be increased without deteriorating the corrosion resistance. However, if the content exceeds 0.20%, the corrosion resistance decreases, so the upper limit for inclusion is 0.20%.
- Cr-containing austenitic alloys C: 0.15% or less, Si: 1.00% or less, Mn: 2.0% or less, P: 0.030% or less, S: 0.030% or less, Cr: 10.0-40.0%, Ni: 45.0-
- a nickel-base alloy containing 80.0%, Ti: 0.5% or less, Cu: 0.5% or less, and Al: 0.5% or less, with the balance being Fe and impurities is preferable. This is because the corrosion resistance is more excellent.
- the above alloy (a) contains 14.0 to 17.0% of Cr and 70 to 80% of Ni, and therefore has excellent corrosion resistance in an environment containing chloride.
- the content of Fe is preferably 6.0 to 10.0% from the viewpoint of the balance between the Ni content and the Cr content.
- the alloy (b) contains 27.0 to 31.0% Cr and 55 to 65% Ni. Therefore, it is excellent in corrosion resistance in high-temperature pure water and alkaline environments as well as in chloride-containing environments.
- the Fe content is preferably 7.0 to 11.0% from the viewpoint of the balance between the Ni content and the Cr content.
- a Cr-containing austenitic alloy tube having a predetermined chemical composition is melted into an ingot. Usually, it is manufactured by a hot working-annealing process or a hot working-cold working-annealing process. Furthermore, in order to improve the corrosion resistance of the base material, a special heat treatment called TT treatment (Thermal Treatment) may be performed.
- TT treatment Thermal Treatment
- the heat treatment method of the present invention may be performed after the above-mentioned annealing or may be performed also as annealing. If annealing is performed, it is not necessary to add a heat treatment process for forming an oxide film in addition to the conventional manufacturing process, and the manufacturing cost is not increased. Further, as described above, when the TT treatment is performed after annealing, this may be performed in combination with the heat treatment for forming the oxide film. Furthermore, both the annealing and the TT treatment may be used as the oxide film forming treatment.
- the resulting tube was heated while moving the tube in a heating furnace while supplying an atmospheric gas at a predetermined flow rate through a header, thereby forming a chromium oxide film on the inner surface of the tube.
- the average film thickness of the examples of the present invention is in the range of 0.05 to 1.5 ⁇ m, and the film thickness distribution is also in a predetermined range. It can be seen that by adjusting the flow rate of the atmospheric gas and the water vapor concentration to the prescribed ranges of the present invention, an appropriate film thickness range and distribution can be obtained even with the water vapor treatment. In particular, when the flow rate of the atmospheric gas is 6.0 L / min or more, it is possible to form an oxide film having a predetermined film thickness and thickness distribution in a wide range of water vapor concentrations.
- FIG. 1 shows the results of C concentration distribution by GDS of Experiment No. 1 and No. 3 and comparative experiment.
- the above-mentioned austenitic alloy tube was treated with hydrogen containing 5600ppm of carbon dioxide gas at a flow rate of 9.0L / min at a heating time of 1100 ° C and a holding time of 5 minutes to form a chromium oxide film on the surface. I let you.
- the C average concentration is 0.013% in the range of 5 to 10 ⁇ m deep from the surface layer portion on the inner surface side, which is less than 0.019% of the base material concentration.
- the C average concentration in the surface layer portion was 0.027%, which was higher than the base material concentration of 0.019%. If C is present in excess of the concentration of the base material contained to increase the grain boundary strength, the possibility of stress corrosion cracking increases. In the steam treatment, the C concentration is moderately reduced near the surface and can be used more safely as a product material.
- the average film thickness of the obtained chromium oxide film was in the range of 0.05 to 1.5 ⁇ m, and the film thickness distribution was also in the predetermined range.
- a Cr-containing austenitic alloy pipe provided with a Cr oxide film having an appropriate film thickness range and distribution within a pipe inner diameter range of 10 to 30 mm can be produced.
- a chromium oxide film that falls within the prescribed range of the present invention can be applied to the inside of the tube even when the tube length is as long as 30 m. Can be formed.
- An alloy tube (tube length: 20 m, tube diameter: 17 mm) having the components shown in Table 4 was oxidized with water vapor to form a chromium oxide film.
- the conditions for forming the film were the same as in Experiment No. 5, in which hydrogen containing 3960 ppm of water was supplied at an air flow rate of 12 L / min, the heat treatment temperature was 1100 ° C., and the treatment time was 5 minutes.
- Table 5 shows the measurement results of the film thickness and C concentration of the treated sample.
- the alloys B, C and D gave almost the same results in both the thickness and distribution of the coating. Moreover, it was confirmed that the C average concentration in the surface layer portion was lower than the C concentration of the base material in the alloy of any component.
- a Cr-containing austenitic alloy tube in which a chromium oxide film is uniformly and inexpensively formed on the inner surface of the tube, and is long in a high-temperature water environment, for example, a high-temperature water environment in a nuclear power plant. Even if it is used for a long time, the elution of Ni is extremely small, so it is most suitable for members used in high-temperature water such as steam generator tubes, especially for nuclear power plants.
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Abstract
Description
0.4≦δ1/δ2≦2.5 ・・・(i)
ただし、δ1、δ2は管の両端それぞれにおけるクロム酸化物皮膜の厚さ(μm)である。
0.4≦δ1/δ2≦2.5 ・・・(i)
ただし、δ1、δ2は管の両端それぞれにおけるクロム酸化物皮膜の厚さ(μm)である。
耐Ni溶出性は、クロム酸化物皮膜の厚さに依存するので、皮膜厚さを制御する必要がある。皮膜厚さは、0.05μm未満では耐Ni溶出性は不十分である。皮膜厚さは0.05μm以上で十分な耐食性を発揮するが、0.1μm以上であることが好ましい。一方、Ni含有量が40%を超えるような高Ni合金では、皮膜厚さを0.2μm以上とすることがより好ましく、0.3μm以上とすることがさらに好ましい。
管の長手方向における皮膜厚さのばらつきが大きく、局部的に厚さの薄い皮膜が形成されると、その部分でNi溶出量が多くなる。そのため、皮膜厚さのばらつきは小さい方がよい。即ち、クロム酸化物皮膜の厚さは、下記(i)式で規定される関係を満足することとする。
0.4≦δ1/δ2≦2.5 ・・・(i)
ただし、δ1、δ2は管の両端それぞれにおけるクロム酸化物皮膜の厚さ(μm)である。
0.5≦δ1/δ2≦2.0
とするのが好ましく、
0.70≦δ1/δ2<1.55
とするのがより好ましい。
本発明の含Crオーステナイト合金管の製造方法では、含Crオーステナイト合金管を、水蒸気および非酸化性ガスからなる雰囲気ガスで加熱することにより、含Crオーステナイト合金管内面にクロム酸化物皮膜を形成させる。
水蒸気は、微量でも含まれておれば、クロム酸化物皮膜を形成するため、特に下限を定めないが、250ppm以上含まれる場合にその効果が顕著となる。水蒸気の濃度の上限については、特に限定しないが、製造コストを低減させる観点からは、25000ppm以下とするのが好ましい。
管の内面に供給する雰囲気ガスの流量は6.0~50L/分とするのが好ましい。6.0L/分未満では、水蒸気濃度や加熱条件を調整しても所望の厚さの酸化物皮膜を形成できない。一方、50L/分を超えると逆に酸化物皮膜が過度に厚くなってしまう。
本発明で規定する水蒸気濃度、熱処理条件で製造した含Crオーステナイト合金管は、管の長さが5~50m、管の内径が10~30mmである原子力プラント用の蒸気発生器用伝熱管に好適である。
加熱処理温度および加熱処理時間については特に制限はないが、例えば、加熱温度は800~1200℃の範囲、加熱時間は1分以上の範囲とすることができる。それぞれの限定理由は下記の通りである。
加熱温度は、適切な酸化物皮膜の厚さおよび組成ならびに合金の強度特性を得ることができる範囲であればよい。具体的には、加熱温度が800℃未満の場合、クロムの酸化が不十分となる場合がある。適正な膜厚を持った皮膜を適正時間で得るには、900℃以上が好ましい。より好ましくは1000℃以上である。一方、上限は1200℃とする。1200℃を超えると、含Crオーステナイト合金管材の強度を確保できなくなるおそれがある。従って、加熱温度は800~1200℃の範囲とするのがよい。
加熱時間は、適切な酸化物皮膜の厚さと組成を得ることができる範囲で設定すればよい。即ち、クロム酸化物を主体とする酸化物皮膜を形成するためには、1分以上加熱することが望ましい。上限は特に定めないが、少なくとも本発明で好ましい温度範囲800~1200℃の範囲では24時間を超えて加熱しても、酸化物皮膜はほとんど生成せず、製造コスト面からも不利となる。従って、加熱時間は1分~24時間の範囲とするのがよい。
本発明の製造方法に供される含Crオーステナイト合金管の素管の化学組成としては、例えば、質量%で、C:0.15%以下、Si:1.00%以下、Mn:2.0%以下、P:0.030%以下、S:0.030%以下、Cr:10.0~40.0%、Ni:8.0~80.0%、Ti:0.5%以下、Cu:0.6%以下、Al:0.5%以下およびN:0.20%以下を含有し、残部がFeおよび不純物からなるものがよい。
Cは、0.15%を超えて含有させると、耐応力腐食割れ性が劣化するおそれがある。従って、Cを含有させる場合には、その含有量を0.15%以下にするのが望ましい。さらに望ましいのは、0.06%以下である。なお、Cは、合金の粒界強度を高める効果を有する。この効果を得るためにはCの含有量は0.01%以上とするのが望ましい。
Siは製錬時の脱酸材として使用され、合金中に不純物として残存する。このとき、1.00%以下に制限するのがよい。その含有量が0.50%を超えると合金の清浄度が低下することがあるため、Si含有量は0.50%以下に制限するのがより望ましい。
Mnは、2.0%を超えると合金の耐食性を低下させるので、2.0%以下とするのが望ましい。さらに望ましいのは、1.0%以下である。Mnは、Crに比べて酸化物の生成自由エネルギーが低く、加熱によりMnCr2O4として析出する。また、拡散速度も比較的早いため、通常は、加熱により母材近傍にCr2O3が優先的に生成し、その外側に上層としてMnCr2O4が形成される。MnCr2O4層が存在すれば、使用環境中においてCr2O3層が保護され、また、Cr2O3層が何らかの理由で破壊された場合でもMnCr2O4によりCr2O3の修復が促進される。このような効果が顕著となるのは、0.1%以上含有させた場合である。
Pは合金中に不純物として存在する元素である。その含有量が0.030%を超えると耐食性に悪影響を及ぼすことがある。従って、P含有量は0.030%以下に制限するのが望ましい。
Sは合金中に不純物として存在する元素である。その含有量が0.030%を超えると耐食性に悪影響を及ぼすことがある。従って、S含有量は0.030%以下に制限するのが望ましい。
Crは、クロム酸化物からなる酸化物皮膜を生成させるために必要な元素である。合金表面にそのような酸化物皮膜を生成させるためには、10.0%以上含有させるのが望ましい。しかし、40.0%を超えると加工性が劣化するおそれがある。従って、Crの含有量は10.0~40.0%が望ましい。
Niは、含Crオーステナイト合金の耐食性を確保するために必要な元素であり、8.0%以上含有させるのが望ましい。一方、Niは高価であるため、用途に応じて必要最小限含有させれば良く、80.0%以下とするのが望ましい。
Tiは、その含有量が0.5%を超えると、合金の清浄性を劣化させるおそれがあるので、その含有量は0.5%以下とするのが望ましい。さらに望ましいのは、0.4%以下である。但し、合金の加工性向上および溶接時における粒成長の抑制の観点からは、0.1%以上含有させることが望ましい。
Cuは合金中に不純物として存在する元素である。その含有量が0.6%を超えると合金の耐食性が低下することがある。従って、Cu含有量は0.6%以下に制限するのが望ましい。
Alは製鋼時の脱酸材として使用され、合金中に不純物として残存する。残存したAlは、合金中で酸化物系介在物となり、合金の清浄度を劣化させ、合金の耐食性および機械的性質に悪影響を及ぼすおそれがある。従って、Al含有量は0.5%以下に制限するのが望ましい。
Nは、添加しなくてもよいが、本発明が対象とする含Crオーステナイト合金中には、通常、0.01%程度のNが不純物として含有されている。しかし、Nを積極的に添加すれば、耐食性を劣化させることなく、強度を高めることができる。ただし、0.20%を超えて含有させると耐食性が低下するので、含有させる場合の上限は0.20%とする。
本発明が対象とする含Crオーステナイト合金管の素管の製造方法としては、所定の化学組成の含Crオーステナイト合金管を溶製してインゴットとした後、通常、熱間加工-焼きなましの工程、または、熱間加工―冷間加工―焼きなましの工程で製造される。さらに、母材の耐食性を向上させるため、TT処理(Thermal Treatment)と呼ばれる特殊熱処理が施されることもある。
Claims (10)
- 含Crオーステナイト合金管の内表面に、厚さが0.05~1.5μmであり、かつ下記(i)式で規定される関係を有するクロム酸化物皮膜を形成した含Crオーステナイト合金管であって、管内面側の表層部より深さ5~10μmの範囲内におけるC平均濃度が、母材のC濃度未満であることを特徴とする含Crオーステナイト合金管。
0.4≦δ1/δ2≦2.5 ・・・(i)
ただし、δ1、δ2は管の両端それぞれにおけるクロム酸化物皮膜の厚さ(μm)である。 - 管の長さが5~50mで、かつ管の内径が10~30mmであることを特徴とする請求項1に記載の含Crオーステナイト合金管。
- 含Crオーステナイト合金管が、質量%で、C:0.15%以下、Si:1.00%以下、Mn:2.0%以下、P:0.030%以下、S:0.030%以下、Cr:10.0~40.0%、Ni:8.0~80.0%、Ti:0.5%以下、Cu:0.6%以下、Al:0.5%以下およびN:0.20%以下を含有し、残部がFeおよび不純物からなることを特徴とする請求項1または請求項2に記載の含Crオーステナイト合金管。
- 含Crオーステナイト合金管が、原子力プラント用部材として用いられることを特徴とする請求項1から請求項3までのいずれかに記載の含Crオーステナイト合金管。
- 含Crオーステナイト合金管の内面に、水蒸気を含有した非酸化性ガスを流通させて加熱し、含Crオーステナイト合金管の内表面に、厚さが0.05~1.5μmで、かつ下記(i)式で規定される関係を満足するクロム酸化物皮膜を形成することを特徴とする含Crオーステナイト合金管の製造方法。
0.4≦δ1/δ2≦2.5 ・・・(i)
ただし、δ1、δ2は管の両端それぞれにおけるクロム酸化物皮膜の厚さ(μm)である。 - 水蒸気を250~25000ppmを含有した非酸化性ガスを6.0~50L/分の範囲で管内に流通させながら800~1200℃の温度範囲において1分以上保持する条件で加熱することを特徴とする請求項5に記載の含Crオーステナイト合金管の製造方法。
- 含Crオーステナイト合金管が、管内面側の表層部より深さ5~10μmの範囲内におけるC平均濃度が、母材のC濃度未満であることを特徴とする請求項5または請求項6に記載の含Crオーステナイト合金管の製造方法。
- 管の長さが5~50mで、かつ管の内径が10~30mmであることを特徴とする請求項5から請求項7までのいずれかに記載の含Crオーステナイト合金管の製造方法。
- 含Crオーステナイト合金管が、質量%で、C:0.15%以下、Si:1.00%以下、Mn:2.0%以下、P:0.030%以下、S:0.030%以下、Cr:10.0~40.0%、Ni:8.0~80.0%、Ti:0.5%以下、Cu:0.6%以下、Al:0.5%以下およびN:0.20%以下を含有し、残部がFeおよび不純物からなることを特徴とする請求項5から請求項8までのいずれかに記載の含Crオーステナイト合金管の製造方法。
- 含Crオーステナイト合金管が、原子力プラント用部材として用いられることを特徴とする請求項5から請求項9までのいずれかに記載の含Crオーステナイト合金管の製造方法。
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KR1020137006687A KR101516505B1 (ko) | 2010-08-26 | 2011-08-12 | Cr함유 오스테나이트 합금관 및 그 제조 방법 |
KR1020157006551A KR101589008B1 (ko) | 2010-08-26 | 2011-08-12 | Cr함유 오스테나이트 합금관 및 그 제조 방법 |
JP2011534850A JP4978755B2 (ja) | 2010-08-26 | 2011-08-12 | 含Crオーステナイト合金管およびその製造方法 |
EP11819808.4A EP2610362B1 (en) | 2010-08-26 | 2011-08-12 | Cr-containing austenite alloy tube |
KR1020167001075A KR101733940B1 (ko) | 2010-08-26 | 2011-08-12 | Cr함유 오스테나이트 합금관 및 그 제조 방법 |
US13/819,072 US9255319B2 (en) | 2010-08-26 | 2011-08-12 | Cr-containing austenitic alloy tube and method for producing the same |
CA2807525A CA2807525C (en) | 2010-08-26 | 2011-08-12 | Cr-containing austenitic alloy tube and method for producing the same |
ES11819808.4T ES2654212T3 (es) | 2010-08-26 | 2011-08-12 | Tubo de aleación de austenita que contiene Cr |
CN201180040742.1A CN103080364B (zh) | 2010-08-26 | 2011-08-12 | 含Cr奥氏体合金管及其制造方法 |
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CN108700285B (zh) * | 2015-11-24 | 2020-07-28 | 法马通公司 | 蒸汽发生器和对应的制造和使用的方法 |
CA3028948C (en) * | 2016-06-28 | 2021-05-11 | Nippon Steel & Sumitomo Metal Corporation | Austenitic alloy material and austenitic alloy pipe |
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WO2013146034A1 (ja) | 2012-03-28 | 2013-10-03 | 新日鐵住金株式会社 | 含Crオーステナイト合金およびその製造方法 |
JP5488762B2 (ja) * | 2012-03-28 | 2014-05-14 | 新日鐵住金株式会社 | 含Crオーステナイト合金およびその製造方法 |
US9695486B2 (en) | 2012-03-28 | 2017-07-04 | Nippon Steel & Sumitomo Metal Corporation | Cr-containing austenitic alloy and method for producing the same |
WO2013150947A1 (ja) | 2012-04-04 | 2013-10-10 | 新日鐵住金株式会社 | クロム含有オーステナイト合金 |
CN104271790A (zh) * | 2012-04-04 | 2015-01-07 | 新日铁住金株式会社 | 含铬奥氏体合金 |
US9493860B2 (en) | 2012-04-04 | 2016-11-15 | Nippon Steel & Sumitomo Metal Corporation | Chromium-containing austenitic alloy |
KR20170003709A (ko) | 2012-04-04 | 2017-01-09 | 신닛테츠스미킨 카부시키카이샤 | 크롬 함유 오스테나이트 합금 |
KR101996712B1 (ko) * | 2012-04-04 | 2019-07-04 | 닛폰세이테츠 가부시키가이샤 | 크롬 함유 오스테나이트 합금 |
WO2013191202A1 (ja) | 2012-06-20 | 2013-12-27 | 新日鐵住金株式会社 | オーステナイト合金管 |
KR20150012288A (ko) | 2012-06-20 | 2015-02-03 | 신닛테츠스미킨 카부시키카이샤 | 오스테나이트 합금관 |
US9859026B2 (en) | 2012-06-20 | 2018-01-02 | Nippon Steel & Sumitomo Metal Corporation | Austenitic alloy tube |
JP2019502021A (ja) * | 2015-12-23 | 2019-01-24 | ポスコPosco | シワ抵抗性に優れたオーステナイト系ステンレス鋼管 |
Also Published As
Publication number | Publication date |
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EP2610362B1 (en) | 2017-10-11 |
JP4978755B2 (ja) | 2012-07-18 |
CA2807525A1 (en) | 2012-03-01 |
US20130206272A1 (en) | 2013-08-15 |
KR20160013254A (ko) | 2016-02-03 |
KR20130061729A (ko) | 2013-06-11 |
CN103080364B (zh) | 2015-02-25 |
KR101733940B1 (ko) | 2017-05-08 |
KR20150036820A (ko) | 2015-04-07 |
CN103080364A (zh) | 2013-05-01 |
US9255319B2 (en) | 2016-02-09 |
KR101516505B1 (ko) | 2015-05-04 |
ES2654212T3 (es) | 2018-02-12 |
KR101589008B1 (ko) | 2016-01-28 |
CA2807525C (en) | 2015-02-03 |
JPWO2012026344A1 (ja) | 2013-10-28 |
EP2610362A4 (en) | 2014-05-07 |
EP2610362A1 (en) | 2013-07-03 |
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