WO2016052445A1 - 二相合金、該二相合金を用いた製造物、および該製造物の製造方法 - Google Patents
二相合金、該二相合金を用いた製造物、および該製造物の製造方法 Download PDFInfo
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- WO2016052445A1 WO2016052445A1 PCT/JP2015/077398 JP2015077398W WO2016052445A1 WO 2016052445 A1 WO2016052445 A1 WO 2016052445A1 JP 2015077398 W JP2015077398 W JP 2015077398W WO 2016052445 A1 WO2016052445 A1 WO 2016052445A1
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/11—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of chromium or alloys based thereon
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/102—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by bonding of conductive powder, i.e. metallic powder
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
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- C21D2211/00—Microstructure comprising significant phases
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/005—Ferrite
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/04—Soldering or other types of metallurgic bonding
- H05K2203/0425—Solder powder or solder coated metal powder
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Definitions
- the present invention relates to a technology for a high corrosion resistance and high strength alloy, and in particular, relates to a two-phase alloy in which two phases of an austenite phase and a ferrite phase are mixed, a product using the two-phase alloy, and a method for producing the product. Is.
- SUS420 is susceptible to stress corrosion cracking (SCC) in an environment containing chloride and acidic gas (for example, carbon dioxide gas or hydrogen sulfide). For this reason, when drilling oil wells in such a severe corrosive environment, expensive nickel (Ni) -based alloys (for example, alloys containing 40% by mass or more of Ni) are often used in the past, and material costs (and therefore drilling costs) ) would rise significantly.
- SCC stress corrosion cracking
- Patent Document 1 Japanese Patent Laid-Open No. 04-3010408
- Patent Document 2 Japanese Patent Laid-Open No. 04-301049 discloses a heat-resistant alloy having a chemical composition consisting of Cr: 70 to 95%, N: 0.1 to 1.5%, the balance Fe and an impurity. It is disclosed.
- Patent Documents 1 and 2 it has excellent compression deformation resistance, oxidation resistance, etc. in a high-temperature atmosphere furnace, improved durability as a heated steel material support surface member, reduced maintenance, and associated furnace operation efficiency. It is said to contribute greatly to improvement.
- Patent Document 3 Japanese Patent Application Laid-Open No. 08-291355 contains, by mass%, Cr: more than 95%, N: 0.1-2.0% by weight, the balance of one or more of Fe, Ni and Co and unavoidable impurities.
- a Cr-based heat-resistant alloy further containing 0.3% or more in total of one or more of Ti, Al, Zr, Nb, B, and V as desired is disclosed.
- Patent Document 3 it is said that a Cr-based heat-resistant alloy excellent in high-temperature strength used for a member that requires strength, ductility, and corrosion resistance at an ultra-high temperature (for example, a heated steel material support member in a heating furnace) can be provided. ing.
- Patent Document 4 Japanese Patent Laid-Open No. 07-258801 discloses that Cr: 15-50%, Ni: 6.1-50%, O + P + S: 200 ppm or less, the balance being Fe and unavoidable impurities, crystal grain size number: 8 As described above, an Fe—Cr—Ni alloy excellent in corrosion resistance of a processed portion, characterized by C + N: 400 to 1200 ppm, if desired, is disclosed. According to Patent Document 4, it is said that an Fe—Cr—Ni alloy can be provided which improves the corrosion resistance without reducing the workability and does not decrease the corrosion resistance even if processed.
- High Cr-based alloys (alloys with a high Cr content) as described in Patent Documents 1 to 3 are intended for use in a high temperature environment of 1300 ° C. or higher, and are excellent even in the high temperature environment. Corrosion resistance and mechanical properties. However, such a high Cr-based alloy exhibits brittleness (insufficient toughness) in the temperature range of the oil well environment (room temperature to about 300 ° C.), and is therefore not considered suitable as an oil well equipment material.
- the Fe—Cr—Ni alloy described in Patent Document 4 is intended for austenitic stainless steel, but austenitic stainless steel is stress-corrosion caused by hydrogen embrittlement in a high temperature and high pressure environment containing chloride. It is known that cracking (SCC) is likely to occur, and it is considered that it is not suitable as an oil well equipment material, as is the case with high Cr-based alloys.
- SCC cracking
- an object of the present invention is a metal material that can be suitably used even in a temperature range and highly corrosive environment such as an oil well, and has a high corrosion resistance equal to or higher than conventional ones and good mechanical properties, and is low in cost. It is an object to provide a two-phase alloy, a product using the two-phase alloy, and a method for producing the product.
- One aspect of the present invention is a two-phase alloy in which Cr (chromium) is a main component and two phases of an austenite phase and a ferrite phase are mixed, and the chemical composition of the two-phase alloy is 34 mass% or more and 70 Cr (mass%) or less, Ni (nickel) of 17 mass% or more and 45 mass% or less, Fe (iron) of 10 mass% or more and 35 mass% or less, and Mn (manganese) of 0.1 mass% or more and 2 mass% or less
- An alloy is provided.
- the present invention can be modified or changed as follows in the above-described two-phase alloy (I) according to the present invention.
- C carbon
- N nitrogen
- O oxygen
- V vanadium
- Nb niobium
- Ta tantalum
- Ti titanium
- Another aspect of the present invention provides a product using a two-phase alloy, wherein the two-phase alloy is the two-phase alloy described above. Is.
- the present invention can add the following improvements and changes to the above-described two-phase alloy product (II) according to the present invention.
- the product is a molded body having a forged structure.
- the product is a composite in which a coating layer of the two-phase alloy is formed on a base material.
- the ratio of the average Cr concentration of the austenite phase to the average Cr concentration of the ferrite phase in the coating layer is 1.3 or less.
- the coating layer has a rapidly solidified structure.
- the product is a rotating machine shaft or bearing.
- the product is a powder.
- the product is a rod-like body or a linear body.
- the product is a welding material.
- the product is a welded joint in which alloy members are welded to each other via a weld, and the weld is made of the two-phase alloy.
- the ratio of the average Cr concentration of the austenite phase to the average Cr concentration of the ferrite phase in the weld is 1.3 or less.
- the alloy member is made of the two-phase alloy.
- Still another embodiment of the present invention is a method for producing the above two-phase alloy product, A raw material mixing and dissolving step for mixing and dissolving raw materials; A casting process for casting to form an ingot; A hot forging process for forming the compact by hot forging the ingot; And a solution heat treatment step of performing a solution treatment in a temperature range of 1050 ° C. or more and 1250 ° C. or less on the formed body.
- the present invention can be improved or changed as follows in the method (III) for producing a two-phase alloy product according to the present invention.
- (Xv) It further has an aging heat treatment step of performing an aging treatment in the temperature range of 800 ° C. or higher and 1000 ° C. or lower on the solution-treated molded body after the solution heat treatment step.
- Still another embodiment of the present invention is a method for producing the above-described two-phase alloy product, A raw material mixing and melting step of mixing and melting the raw materials of the two-phase alloy to form a molten metal; An atomizing step of forming alloy powder from the molten metal;
- the present invention provides a method for producing a two-phase alloy product, comprising: a layered manufacturing process for forming a coating layer of the two-phase alloy on the base material using the alloy powder.
- Still another embodiment of the present invention is a method for producing the above-mentioned two-phase alloy product, A raw material mixing and melting step of mixing and melting the raw materials of the two-phase alloy; A casting process for casting to form an ingot; A hot working forming step of hot working the ingot to form a rod-like body or a linear body; and
- the present invention provides a method for producing a two-phase alloy product, comprising a welding step of welding the alloy members using the rod-like body or linear body as a welding material.
- the metal material As a metal material that can be suitably used even in a temperature range and highly corrosive environment such as an oil well, the metal material has high corrosion resistance equal to or higher than that of conventional ones and good mechanical properties, and is low in cost.
- a two-phase alloy, a product using the two-phase alloy, and a method for producing the product can be provided.
- the inventors of the present invention used a Cr—Ni—Fe alloy containing Cr as a main component, particularly a Cr—Ni—Fe alloy containing 34 mass% or more of Cr, a composition, a metallographic form, and a product using the alloy.
- the present invention was completed by intensive investigation and examination on the relationship between mechanical properties and corrosion resistance.
- the alloy of the present invention is a Cr—Ni—Fe alloy containing Cr, Ni and Fe as main components.
- the metal structure of an alloy containing Fe as a main component is usually a ferrite structure having a body-centered cubic lattice crystal structure (also referred to as a ferrite phase or ⁇ phase) and an austenite structure having a face-centered cubic lattice crystal structure (austenite phase). , Also referred to as a ⁇ phase), and a martensite structure having a distorted body-centered cubic lattice crystal structure (also referred to as a martensite phase or an ⁇ ′ phase).
- the ferrite phase has excellent corrosion resistance (for example, SCC resistance) and high mechanical strength (for example, 0.2% proof stress), but it is said that the ductility and toughness are relatively low compared to the austenite phase. ing.
- the austenite phase has relatively high ductility and toughness compared to the ferrite phase, but is considered to have relatively low mechanical strength.
- high corrosion resistance is shown in a normal environment, when the corrosive environment becomes severe, it is said that SCC resistance will fall rapidly.
- the martensite phase has high mechanical strength (for example, hardness), but is considered to have relatively low corrosion resistance.
- the two-phase alloy according to the present invention is an alloy in which two phases of an austenite phase and a ferrite phase are mixed as a metal structure.
- Two-phase alloys are characterized by combining the advantages of an austenite phase (excellent ductility and toughness) with the advantages of a ferrite phase (high mechanical strength and excellent corrosion resistance including SCC resistance). Further, since Cr, which is cheaper than Ni, is used as a main component, there is an advantage that material costs can be reduced as compared with a Ni-based alloy having Ni as the maximum component.
- the occupancy ratio of the ferrite phase (hereinafter sometimes simply referred to as “ferrite ratio”) is 10% or more and 90% or less, and the balance is the austenite phase.
- the phase occupancy in the present invention is defined as the content (unit:%) of the phase when backscattered electron diffraction image (EBSP) analysis is performed on the polished surface of the alloy bulk sample.
- EBSP backscattered electron diffraction image
- the ferrite ratio is out of the range of 10% or more and 90% or less, the advantage as a two-phase alloy is hardly obtained (the weak point of the austenite phase single phase or the weak point of the ferrite phase single phase appears clearly).
- the ferrite ratio is more preferably 20% or more and 70% or less, and further preferably 30% or more and 70% or less.
- the product made of the two-phase alloy of the present invention preferably has a metal structure (for example, a forged structure or a rapidly solidified structure) having a small crystal grain size from the viewpoint of mechanical properties and corrosion resistance.
- the product is preferably formed and shaped by forging or rapid solidification using the two-phase alloy of the present invention.
- the metal structure may be a metal structure that has been subjected to a solution heat treatment after forging or rapid solidification modeling, or may be a metal structure that has been subjected to an aging heat treatment.
- FIG. 1 is an example of a two-phase alloy material according to the present invention, and is an optical micrograph showing an example of a metal structure of a sample subjected to solution heat treatment after hot forging.
- the two-phase alloy according to the present invention has a metal structure in which a bright austenite phase P1 and a dark ferrite phase P2 are dispersed and mixed with each other.
- a structure in which a cast solidified structure for example, a dendritic crystal peculiar to the cast solidified structure
- an equiaxed crystal grain is seen at least partially (so-called forged structure) ).
- Other details will be described later.
- the two-phase alloy according to the present invention is a Cr—Ni—Fe-based alloy containing Cr, Ni and Fe as main components. Further, it contains at least Mn and Si as subcomponents, additionally contains at least one of V, Nb, Ta and Ti, and further contains impurities.
- the composition (each component) of the two-phase alloy according to the present invention will be described.
- the Cr component is one of the main components of the two-phase alloy, and forms a high-strength ferrite phase and contributes to the improvement of corrosion resistance by forming a solid solution in the austenite phase.
- the Cr component content is preferably 34% by mass to 70% by mass, more preferably 34% by mass to 65% by mass, and still more preferably 40% by mass to 60% by mass. When the Cr content is less than 34% by mass, the ferrite content is less than 10% (the austenite phase occupancy is more than 90%), and the mechanical strength of the two-phase alloy is lowered.
- the Cr content exceeds 70% by mass, the ferrite ratio exceeds 90% (the austenite phase occupancy is less than 10%), and the ductility and toughness of the two-phase alloy are reduced. Further, from the viewpoint of corrosion resistance and material cost, it is preferable that the Cr content is the maximum content among the three main components (Cr, Ni, Fe).
- Ni 17-45% by mass
- the Ni component is one of the main components of this two-phase alloy, and contributes to maintaining the two-phase state of the alloy by stabilizing the austenite phase (for example, the two-phase state is maintained even when solution treatment is performed). It is a component that imparts ductility and toughness to the two-phase alloy.
- the content of the Ni component is preferably 17% by mass or more and 45% by mass or less, and more preferably 20% by mass or more and 40% by mass or less. When the Ni content is less than 17% by mass, the occupancy ratio of the austenite phase is less than 10% (ferrite ratio is more than 90%), and the ductility and toughness of the two-phase alloy are lowered. On the other hand, when the Ni content exceeds 45% by mass, the ferrite ratio becomes less than 10% (the austenite phase occupancy exceeds 90%), and the mechanical strength of the two-phase alloy decreases.
- the Fe component is also one of the main components of this two-phase alloy, and is a basic component for ensuring mechanical strength.
- the content of the Fe component is preferably 10% by mass to 35% by mass, and more preferably 10% by mass to 32% by mass.
- the Fe content is less than 10% by mass, the ductility and toughness of the two-phase alloy are lowered.
- the Fe content exceeds 35% by mass the ⁇ phase of the intermetallic compound is likely to be generated in the temperature range near 800 ° C., and the ductility and toughness of the two-phase alloy are significantly reduced (so-called ⁇ phase embrittlement). ).
- ⁇ phase embrittlement the ductility and toughness of the two-phase alloy
- Ni + Fe 30-65 mass%
- the total content of the Ni component and the Fe component is preferably 30% by mass to 65% by mass, more preferably 40% by mass to 62% by mass, and still more preferably 45% by mass to 55% by mass.
- the total content is less than 30% by mass, the ductility / toughness of the two-phase alloy becomes insufficient.
- the total content exceeds 65% by mass, the mechanical strength is greatly reduced.
- Mn 0.1-2% by mass
- the Mn component plays a role of desulfurization and deoxidation in this two-phase alloy, and is a subcomponent that contributes to improvement of mechanical strength and toughness and improvement of carbon dioxide gas corrosion resistance.
- the content of the Mn component is preferably 0.1% by mass or more and 2% by mass or less, and more preferably 0.3% by mass or more and 1.8% by mass or less. When the Mn content is less than 0.1% by mass, the effect of the Mn component cannot be sufficiently obtained. On the other hand, when the Mn content exceeds 2 mass%, coarse particles of sulfide (for example, MnS) are formed, which causes deterioration of corrosion resistance and mechanical strength.
- MnS coarse particles of sulfide
- the Si component plays a role of deoxidation in the present two-phase alloy and is a subcomponent that contributes to improvement of mechanical strength and toughness.
- the content of the Si component is preferably 0.1% by mass or more and 1% by mass or less, and more preferably 0.3% by mass or more and 0.8% by mass or less. When the Si content is less than 0.1% by mass, the effect of the Si component cannot be sufficiently obtained. On the other hand, when the Si content exceeds 1% by mass, coarse particles of oxide (for example, SiO 2 ) are formed, which causes a decrease in toughness.
- Impurities in this two-phase alloy include P, S, C, N, and O. Hereinafter, these impurities will be described.
- the P component is an impurity component that easily segregates at the crystal grain boundaries of the two-phase alloy and lowers the toughness of the alloy and the corrosion resistance of the grain boundaries.
- the P content is more preferably 0.03% by mass or less.
- S component more than 0% by mass and 0.01% by mass or less
- S component is easy to form a relatively low melting point sulfide (for example, Fe sulfide) by combining with the components of this two-phase alloy, and the toughness and pore resistance of the alloy It is an impurity component that lowers food habits.
- the S content is more preferably 0.003% by mass or less.
- C More than 0% by mass and 0.03% by mass or less C component has the effect of hardening the alloy by solid solution, but combines with the components of this two-phase alloy to produce carbide (for example, Cr carbide). It is also an impurity component that easily precipitates at grain boundaries and lowers the corrosion resistance and toughness of the alloy.
- carbide for example, Cr carbide
- the C content is more preferably 0.02% by mass or less.
- N component more than 0% by mass and 0.02% by mass or less N component has the effect of hardening the alloy by solid solution, while it combines with the components of this two-phase alloy to form nitride (eg Cr nitride) It is also an impurity component that easily forms and precipitates and lowers the toughness of the alloy.
- the N content is more preferably 0.015% by mass or less.
- O component is an impurity component that easily forms and precipitates an oxide (for example, Fe oxide) by combining with the constituent components of this two-phase alloy and lowers the toughness of the alloy. is there.
- oxide for example, Fe oxide
- the O content is more preferably 0.02% by mass or less.
- the present two-phase alloy preferably further contains at least one of V, Nb, Ta, and Ti as an additional subcomponent.
- V, Nb, Ta, and Ti as an additional subcomponent.
- the V component, the Nb component, the Ta component, and the Ti component are components that play a role of decarburization, denitrification, and deoxidation in the two-phase alloy, respectively.
- the toughness of the alloy can be improved (decrease in toughness can be suppressed).
- the addition of a small amount of the V component has a secondary effect of improving the mechanical properties (for example, hardness and tensile strength) of the alloy.
- the addition of a small amount of the Nb component also has a secondary effect of improving the mechanical properties (for example, toughness) of the alloy.
- Addition of a small amount of Ta component or Ti component has a secondary effect of improving the corrosion resistance of the alloy.
- the total content of the additional subcomponents is preferably controlled to be in the range of 0.8 to 2 times the total content of impurity components C, N, and O.
- the total content of additional subcomponents is less than 0.8 times the total content of C, N, and O, the above-described effects cannot be obtained sufficiently.
- the total content of additional subcomponents exceeds twice the total content of C, N, and O, the ductility and toughness of the alloy decrease.
- FIG. 2 is a process diagram showing an example of a method for producing a two-phase alloy product according to the present invention.
- the raw material of the two-phase alloy is mixed and melted so as to have a desired composition (main component + subcomponent + optional subcomponent if necessary).
- the raw material mixing dissolution process (step 1: S1) which forms 10 is performed.
- vacuum melting can be suitably used as a melting method.
- step 2 a casting process for casting using a predetermined mold is performed (step 2: S2).
- this casting process A two-phase alloy product according to the present invention may be used as a casting.
- the ingot 20 is once produced.
- a hot forging process (step 3: S3) is performed in which the ingot 20 is hot-forged and formed into a substantially final shape.
- the hot forging / forming method there is no particular limitation on the hot forging / forming method, and a conventional method can be used, but the temperature of hot forging is preferably in the range of 1050 to 1250 ° C.
- a solution heat treatment step for subjecting the forged formed body 30 to a solution treatment may be performed as necessary.
- the temperature of the solution heat treatment is preferably in the range of 1050 to 1150 ° C, more preferably around 1100 ° C.
- step 5 it is preferable to perform an aging heat treatment step (step 5: S5) after the solution heat treatment step S4.
- the temperature of the aging heat treatment is preferably in the range of 800 to 1000 ° C, more preferably around 900 ° C.
- the heat treatment time may be appropriately adjusted within a range of 0.5 to 6 hours.
- the austenite phase when the ferrite phase is more than the expected ferrite ratio from the composition, by applying this aging heat treatment, a part of the ferrite phase is transformed into the austenite phase to adjust the elongation and toughness of the product. be able to.
- the austenite phase is partly transformed into a ferrite phase to adjust the mechanical strength of the product. Can do.
- the two-phase alloy material contains an additional subcomponent
- compound formation of the additional subcomponent and impurity components (C, N, O) simultaneously with the above-mentioned phase ratio adjustment Is promoted, and the impurity components can be more aggregated and stabilized.
- the toughness of the product can be further improved (a decrease in toughness can be further suppressed).
- the product manufactured as described above is made of a two-phase alloy containing Cr as a main component, which is cheaper than Ni, the Ni-based alloy has high corrosion resistance and mechanical properties equal to or higher than conventional ones. Cost reduction can be achieved compared to a product made of an alloy.
- the two-phase alloy product according to the present invention is an oil well equipment member (for example, a rotating machine (compressor, pump, etc.) member (shaft, bearing, etc.)) or seawater environment equipment used in a severe corrosive environment. It can be suitably used as a member (eg, seawater desalination plant equipment member, umbilical cable) or a chemical plant equipment member (eg, liquefied natural gas vaporizer member).
- FIG. 3 is a process diagram showing another example of the method for producing a two-phase alloy product according to the present invention.
- the manufacturing method of FIG. 3 is an example of the manufacturing method of the composite_body
- a raw material for forming a molten metal 10 by mixing and melting raw materials of a two-phase alloy so as to have a desired composition (main component + subcomponent + additional subcomponent if necessary).
- a mixing dissolution process (step 1: S1) is performed.
- vacuum melting can be suitably used as a melting method.
- an atomizing process for forming the alloy powder 40 from the molten metal 10 is performed (step 6: S6).
- the atomizing method There is no particular limitation on the atomizing method, and a conventional method can be used.
- a gas atomizing method capable of obtaining highly clean, homogeneous composition and spherical particles can be preferably used.
- the average particle size of the alloy powder 40 is preferably 1 ⁇ m or more and 100 ⁇ m or less from the viewpoint of handling properties and filling properties.
- the obtained alloy powder 40 can be the two-phase alloy product of the present invention even in this state.
- it can be suitably used as a welding material, powder metallurgy material, and additive manufacturing material.
- a layered manufacturing process (step 7: S7) is performed in which the alloy powder 40 prepared above is used to form a coating layer 52 of a two-phase alloy on a predetermined substrate 51.
- the additive manufacturing method is not particularly limited, and a conventional method can be used.
- a metal powder additive manufacturing method using electron beam irradiation heating or laser irradiation heating can be suitably used.
- the additive manufacturing process includes an alloy powder deposition process in which a deposited layer of the alloy powder 40 is formed on the substrate 51, and a locally molten layer of the alloy is formed by locally heating the deposited layer.
- a solution heat treatment process S4 similar to that in FIG. 2 may be performed as necessary.
- the chemical composition can be homogenized in each phase of the austenite phase and the ferrite phase.
- a hot isostatic pressing (HIP) method may be employed. By performing hot isostatic pressing, the solidified structure of the two-phase alloy coating layer 52 can be further densified, or defects in the solidified structure can be eliminated.
- an aging heat treatment step S5 similar to FIG. 2 may be performed as necessary.
- the phase ratio of the two phases can be adjusted.
- FIG. 4a is a schematic perspective sectional view showing an example of the two-phase alloy coating layer obtained by the present invention
- FIG. 4b is an enlarged schematic view of a part A of FIG. 4a.
- the two-phase alloy coating layer 52 has a metal structure composed of a set of rapidly solidified structures 60 formed by rapid solidification of a micro weld pool due to the additive manufacturing method.
- each rapidly solidified structure 60 has a substantially hemispherical outline derived from the outer edge shape (melting boundary 61) of the micro weld pool by local heating.
- the rapidly solidified structure 60 is arranged in a two-dimensional manner with the arcs directed in the same direction, and a layered solidified layer 62 is formed. Further, a plurality of such solidified layers 62 are laminated in the thickness direction.
- the rapidly solidified structure 60 becomes a metal structure arranged in a three-dimensional manner. Note that the melt boundary 61 may not be clearly observed depending on the conditions of the additive manufacturing method.
- the crystal 65 is growing, and the columnar crystal 65 stands through the large tilt grain boundary 66.
- a small tilt grain boundary 67 may be observed inside each columnar crystal 65.
- a grain boundary having a tilt angle between adjacent crystal grains (a tilt angle between predetermined crystal orientations) of 15 ° or more is defined as a large tilt grain boundary, and a grain boundary less than 15 ° is defined as a low tilt grain boundary.
- the tilt angle of the crystal grain boundary can be measured by backscattered electron diffraction image (EBSP) analysis.
- EBSP backscattered electron diffraction image
- the average crystal grain size of the columnar crystals 65 needs to be at least 100 ⁇ m or less. From the viewpoint of mechanical strength and corrosion resistance of the two-phase alloy material, the average crystal grain size of the columnar crystals 65 is more preferably 50 ⁇ m or less, and further preferably 10 ⁇ m or less.
- the average crystal grain size in the present invention is obtained by reading an optical microscope observation image or an electron microscope observation image with an image analysis software (NIH Image, public domain software), binarizing, and then binarizing the minor axis of the crystal grain And the average value calculated from the major axis.
- the ratio of the average Cr concentration of the austenite phase ( ⁇ phase) to the average Cr concentration of the ferrite phase ( ⁇ phase) “(Cr concentration of ⁇ phase)” / (Cr concentration of ⁇ phase) ”(referred to as solid-liquid partition coefficient) was investigated using an electron beam probe microanalyzer (EPMA), and the ratio (solid-liquid partition coefficient) was 1.3 or less. And it has been confirmed that the two-phase alloy material having such a composition ratio exhibits higher corrosion resistance than the two-phase alloy material having the composition ratio (solid-liquid distribution coefficient) exceeding 1.3. Details will be described later.
- the two-phase alloy coating layer 52 formed according to the present embodiment exhibits high corrosion resistance, it can be suitably used as a corrosion-resistant coating.
- the product of the present embodiment is an oil well equipment member (for example, a compressor member, a pump) used in a severe corrosive environment. Member), seawater environment equipment member (for example, seawater desalination plant equipment member, umbilical cable) and chemical plant equipment member (for example, liquefied natural gas vaporizer member).
- this embodiment is not limited to it, It combines with a base material using an additive manufacturing method.
- a molded body having a desired shape may be formed without this, and the molded body may be used as a corrosive environment equipment member.
- FIG. 5 is a process diagram showing still another example of the method for producing a two-phase alloy product according to the present invention.
- the manufacturing method shown in FIG. 5 shows that a rod-like material or wire-like material made of the two-phase alloy of the present invention is produced, and the alloy members are welded together using the rod-like material or wire-like material as a welding material.
- the same raw material mixing and dissolving step S1 as in FIG. 2 is performed.
- the method of mixing and melting the raw materials there are no particular limitations on the method of mixing and melting the raw materials, and conventional methods in the production of high corrosion resistance and high strength alloys can be used.
- vacuum melting can be suitably used as a melting method.
- the ingot 20 is produced by performing a casting step S2 similar to FIG.
- a hot working forming step (step 3 ': S3') is performed in which the ingot 20 is hot worked to form a rod-like body or a linear body 70.
- the hot working forming method for forming the rod-like body or linear body 70 and conventional methods (for example, extrusion processing, drawing processing) can be used, but the hot working temperature is 1050 to 1250 ° C. A range is preferred.
- the obtained alloy rod-like body or alloy wire-like body 70 can be the two-phase alloy product of the present invention even in this state.
- it can be suitably used as a welding material.
- a welding step (step 8: S8) is performed in which a predetermined joint member 81 is welded together to form a weld joint 80 using the alloy rod-like body or alloy linear body 70 prepared above.
- a conventional method can be used.
- laser welding, electron beam welding, or arc welding can be suitably used.
- the material of the alloy member 81 to be welded is not particularly limited. However, when the welded product (welded joint 80) is used as a corrosive environment equipment member, the material to be welded is a two-phase alloy material. It is preferable that the two-phase alloy material be the two-phase alloy material of the present invention.
- a solution heat treatment step S4 similar to FIG. 2 may be performed as necessary.
- the chemical composition can be homogenized in each phase of the austenite phase and the ferrite phase.
- an aging heat treatment step S5 similar to FIG. 2 may be performed as necessary.
- the phase ratio of the two phases can be adjusted.
- the welded portion 82 of the welded joint 80 obtained according to the present embodiment has a metal structure composed of a rapidly solidified structure 60 similar to that of FIG. Specifically, it has columnar crystals 65 having an average crystal grain size of 100 ⁇ m or less, and has a microstructure in which the ratio of the average Cr concentration of the ⁇ phase to the average Cr concentration of the ⁇ phase (solid-liquid distribution coefficient) is 1.3 or less.
- the microstructure shows high corrosion resistance as described above, a welded joint 80 with high corrosion resistance can be obtained.
- the product of this embodiment (the welded joint 80 welded via the two-phase alloy welded portion 82 of the present invention) can provide a larger member as a corrosive environmental equipment member.
- invention alloys IA 1 to IA 8 and comparative alloys CA 1 to CA 3 are Cr-based alloys containing Cr as a main component.
- CA1 to CA3 are high Cr-based alloys containing more than 65% by mass of Cr.
- the comparative alloy CA-4 is a Ni-based alloy containing Ni as a main component.
- Comparative alloy CA-5 is a commercially available duplex stainless steel as described above, and is an Fe-based alloy containing Fe as a main component.
- each alloy product (excluding Comparative Example 5) was performed according to the production method shown in FIG. First, the raw materials of each alloy were mixed, and vacuum melting (5 ⁇ 10 ⁇ 3 Pa or lower, 1600 ° C. or higher) was performed using a high-frequency vacuum melting furnace. Next, it casted using the predetermined
- the hot forging conditions for Examples 1 to 14 and Comparative Example 4 were as follows: forging temperature: 1050 to 1250 ° C., strain rate: 8 mm / s or less, rolling reduction per forging: 10 mm or less, number of forgings: 6 times That is all.
- the hot forging conditions for Comparative Examples 1 to 3 are the same as other conditions, but instead of reducing the amount of reduction per forging, the number of forgings is increased so that the total forging deformation amount is the same as that of the invention alloy material. It was.
- the range of the forging temperature is determined as follows. Separately cut and test specimens for tensile test from each ingot, and perform high-temperature tensile tests (test temperature: 800-1350 ° C, tensile speed: 10 mm / s) using a greeble tester. went. As a result of the high-temperature tensile test, the temperature range where the drawing is 60% or more was defined as the forging temperature range.
- Example 5 Each alloy sample subjected to hot forging was subjected to solution heat treatment (held at 1100 ° C. for 60 minutes and then water-cooled). Some samples were alloy products for testing and evaluation in this state (Examples 1, 3, 5, 9, 11 to 14 and Comparative Examples 1 to 4). Further, the same solution heat treatment was performed on the purchased CA-5 sample, and an alloy product for test and evaluation (Comparative Example 5) was obtained.
- An aging heat treatment (holding at 800 to 1000 ° C. for 60 minutes and then water cooling) was applied to the other part of the sample subjected to the solution heat treatment.
- the samples subjected to the aging heat treatment were used as test and evaluation alloy products (Examples 2, 4, 6 to 8, 10).
- Example 5 (Test and evaluation for alloy products of Examples 1 to 14 and Comparative Examples 1 to 5) (1) Microstructure observation After specimens for microstructure observation were collected from each alloy product, the surface of the specimen was mirror-polished and subjected to electric field etching in an oxalic acid aqueous solution. The polished surface was observed with an optical microscope.
- FIG. 1 shown above is an optical micrograph of the metal structure of Example 5.
- the two-phase alloy material of the present invention has a metal structure in which a light austenite phase P1 and a dark ferrite phase P2 are dispersed and mixed with each other. Further, since hot forging is performed, a cast solidification structure (for example, dendritic crystals peculiar to the cast solidification structure) is destroyed, and a structure in which equiaxed crystal grains are observed at least partially (so-called forging) Organization). The other examples were the same.
- Microstructure stability test Samples for microstructural stability test were collected from each alloy product of the examples, and then heat treatment was performed at 800 ° C for 60 minutes. X-ray diffraction measurement was performed on the surface of each test piece, and the presence or absence of the generation of ⁇ phase of the intermetallic compound was investigated. As a result of the investigation, it was confirmed that in all of Examples 1 to 14, no ⁇ phase was detected, and it was difficult to generate the ⁇ phase.
- Room temperature tensile test A specimen for a tensile test (diameter: 4 mm, parallel part length: 20 mm) was taken from each of the prepared alloy products. As another mechanical property evaluation, a room temperature tensile test (strain rate: 3 ⁇ 10 -4 s -1 ) was performed on each specimen using a tensile tester, and 0.2% proof stress, tensile strength, and elongation at break were measured. It was measured. In addition, when the test piece broke before the clear tensile strength was measured, the breaking stress was measured. The results of these tensile tests were determined as the average of 3 measurements.
- Comparative Example 4 (a product made of CA 4) was a Ni-based alloy material as described above, and showed a metal structure of an austenite phase single phase (ferrite ratio 0%). Mechanical strength (Vickers hardness, 0.2% proof stress, tensile strength) was difficult. Moreover, since the content rate of Ni component is high, there exists a difficulty also from a viewpoint of material cost.
- Comparative Example 5 made of commercially available duplex stainless steel (CA-5) had a ferrite rate of 45%.
- Examples 1 to 14 (products comprising IA 1 to IA 8) all had a metal structure of a two-phase alloy in which an austenite phase and a ferrite phase were mixed.
- the ferrite ratio was changed from the examples where the aging heat treatment was not performed. That is, it was confirmed that the aging heat treatment after the solution heat treatment acts as a ferrite ratio adjusting heat treatment.
- Examples 1 to 14 have good properties (for example, Vickers hardness of more than 250 Hv, 0.2% proof stress of more than 550 MPa, tensile strength of more than 900 MPa, rupture of 2% or more. (Elongation) was confirmed.
- Examples 1 to 14 had good mechanical properties equivalent to or better than conventional materials and excellent corrosion resistance. Furthermore, since the content of Cr component is high, it can be said that the cost can be reduced as compared with the conventional Ni-based alloy material.
- the invention alloys IA 9 to IA 17 include additional subcomponents (V, Nb, Ta, Ti) in addition to the main components (Cr, Ni, Fe) and subcomponents (Mn, Si). ).
- the total content of additional subcomponents is in the range of 0.8 to 2 times the total content of C, N and O.
- Each alloy product is manufactured in accordance with the manufacturing method shown in FIG. 1. After the solution heat treatment process (holding at 1100 ° C. for 60 minutes and water cooling), the aging heat treatment process (after holding at 800 to 1050 ° C. for 60 minutes) , Water cooling). The relationship between the alloy number and the heat treatment condition in the alloy products of Examples 15 to 32 is shown in Table 4 described later.
- each of Examples 15 to 32 (products comprising IA 9 to IA 17) is a two-phase alloy in which an austenite phase and a ferrite phase are mixed, as in FIG. It had a metallographic structure. Moreover, the ferrite rate changed with the difference in the temperature of aging heat processing. That is, it was confirmed that the aging heat treatment after the solution heat treatment acts as a ferrite ratio adjusting heat treatment.
- the pitting corrosion occurrence potential corresponding to a current density of 100 ⁇ A / cm 2 is 1.1 V in all samples (Examples 16, 18, 20, 22, 23, 25, 27, and 32) subjected to the pitting corrosion test. As described above, in the region above the pitting potential, oxygen was generated in the hyperpassive region. In all these samples, no pitting corrosion was observed. In the sulfuric acid resistance test, Examples 15 to 32 showed a corrosion current density of 1 to 10% as compared with Comparative Example 5. That is, it was confirmed that Examples 15 to 32 have extremely excellent corrosion resistance.
- Examples 15 to 32 have good properties (for example, Vickers hardness of more than 200vHv, 0.2% proof stress of more than 550 MPa, tensile strength of more than 800 MPa, breakage of 5% or more. (Elongation) was confirmed. In Examples 15 to 32, the elongation at break was significantly improved. This was thought to be due to the fact that the impurities C, N and O were assembled and stabilized by adding additional subcomponents in an appropriate range.
- FIG. 6 is a graph showing the relationship between the ferrite ratio and Vickers hardness in the two-phase alloy product of the present invention
- FIG. 7 shows the relationship between the ferrite ratio and 0.2% proof stress in the two-phase alloy product of the present invention. It is a graph to show.
- the two-phase alloy product comparison was made in Examples 1, 3, 5, 9, 16, 18, 20, and 22 in which the Fe concentration was around 20% by mass.
- the Vickers hardness monotonously increased with the increase of the ferrite ratio, and when the ferrite ratio was larger than 40%, it was found to be approximately 400 mmHv or more.
- the 0.2% proof stress also increased monotonously with the increase of the ferrite ratio, and it was found that when the ferrite ratio was larger than 40%, the yield was generally about 1000 MPa or more.
- the Fe concentration is in the vicinity of 20% by mass, and the ferrite ratio increases as the Cr concentration increases.
- the ferrite ratio increases, and the Vickers hardness and the 0.2% proof stress tend to increase.
- the ferrite phase becomes a single phase as in Comparative Examples 1 to 3, since it is almost ductile and brittle. In other words, it is important to maintain the two-phase mixed state by controlling the ferrite ratio to 90% or less. Further, the addition of additional subcomponents (V, Nb, Ta, Ti) can greatly improve the elongation at break. Whether to give priority to mechanical strength or to ductility may be appropriately selected according to the characteristics required of the two-phase alloy product.
- Examples 33 to 36 of alloy products Using the inventive alloys 1 to 4 (IA 1 to IA 4) shown in Table 1, an alloy powder (average particle size of 100 ⁇ m or less) is prepared according to the manufacturing method shown in FIG. Alloy products (Examples 33 to 36) were prepared by the method. In this experiment, a molded body that was not combined with the base material was modeled.
- Fig. 8a is an optical micrograph showing the metal structure of Example 9
- Fig. 8b is an optical micrograph showing the metal structure of Example 36.
- Example 9 since hot forging is performed, as in Example 5 of FIG. 1, dendritic crystals peculiar to the cast solidification structure are destroyed, and equiaxed crystal grains are seen at least partially. It was confirmed that it has a structure (so-called forged structure).
- Example 36 each of the ⁇ -phase and ⁇ -phase crystal grains was small and more evenly dispersed, and crystal grains like the initial shape of the dendrites were observed. It was confirmed to have.
- Examples 33 to 36 have different ferrite ratios and higher mechanical strength (Vickers hardness) than Examples 1, 3, 5, and 9 having the same alloy composition. , 0.2% proof stress, tensile strength) and ductility equal to or higher than that. These results are thought to be strongly related to the refinement of crystal grains by rapid solidification and the uniform dispersion of ⁇ and ⁇ phases.
- Example 36 was 1.28 smaller than 1.53 of Example 9. This means that the difference between the Cr concentration of the ⁇ phase and the Cr concentration of the ⁇ phase in Example 36 is smaller than that in Example 9, and that Example 36 was produced by rapid solidification. It will be a proof of.
- Examples 33 to 36 each had a higher pitting corrosion generating potential than the corresponding Examples. Although the detailed mechanism of this result has not been elucidated, it is considered that a decrease in the solid-liquid partition coefficient (a decrease in the Cr concentration difference between the ⁇ phase and the ⁇ phase) is involved.
- FIG. 9 is a chart showing the change over time of current density in constant potential polarization of 1000 mV (vs. SHE) in Examples 9 and 36. As shown in FIG. 9, in Example 36, the current density decreases with time, which means that the corrosion rate is lower than that in Example 9. That is, it was confirmed that Example 36 has higher corrosion resistance than Example 9.
Abstract
Description
(i)前記不純物として、0質量%超0.03質量%以下のC(炭素)と、0質量%超0.02質量%以下のN(窒素)と、0質量%超0.03質量%以下のO(酸素)とを含み、前記二相合金の構成成分として、V(バナジウム)、Nb(ニオブ)、Ta(タンタル)およびTi(チタン)のうちの少なくとも一種を更に含み、前記V、Nb、TaおよびTiの合計含有率が、前記C、NおよびOの合計含有率の0.8倍以上2倍以下の範囲である。
(ii)前記不純物として、0質量%超0.04質量%以下のP(リン)と、0質量%超0.01質量%以下のS(硫黄)とを含む。
(iii)前記フェライト相の占有率が10%以上90%以下である。
(iv)前記製造物は、鍛造組織を有する成形体である。
(v)前記製造物は、基材上に前記二相合金の被覆層が形成された複合体である。
(vi)前記被覆層中の前記フェライト相の平均Cr濃度に対する前記オーステナイト相の平均Cr濃度の比率が1.3以下である。
(vii)前記被覆層は、急冷凝固組織を有する。
(viii)前記製造物は、回転機械の軸または軸受である。
(ix)前記製造物は、粉体である。
(x)前記製造物は、棒状体または線状体である。
(xi)前記製造物は、溶接材料である。
(xii)前記製造物は、合金部材同士が溶接部を介して溶接された溶接継手であり、前記溶接部が前記二相合金からなる。
(xiii)前記溶接部における前記フェライト相の平均Cr濃度に対する前記オーステナイト相の平均Cr濃度の比率が1.3以下である。
(xiv)前記合金部材が前記二相合金からなる。
原料を混合・溶解する原料混合溶解工程と、
鋳造して鋳塊を形成する鋳造工程と、
前記鋳塊を熱間鍛造して成形体を形成する熱間鍛造成形工程と、
前記成形体に対して1050℃以上1250℃以下の温度範囲で溶体化処理を施す溶体化熱処理工程とを有することを特徴とする二相合金製造物の製造方法を提供するものである。
(xv)前記溶体化熱処理工程の後に、溶体化処理した前記成形体に対して800℃以上1000℃以下の温度範囲で時効処理を施す時効熱処理工程を更に有する。
前記二相合金の原料を混合・溶解して溶湯を形成する原料混合溶解工程と、
前記溶湯から合金粉末を形成するアトマイズ工程と、
前記合金粉末を用いて前記基材上に前記二相合金の被覆層を形成する積層造形工程とを有することを特徴とする二相合金製造物の製造方法を提供するものである。
前記二相合金の原料を混合・溶解する原料混合溶解工程と、
鋳造して鋳塊を形成する鋳造工程と、
前記鋳塊を熱間加工して棒状体または線状体を形成する熱間加工成形工程と、
前記棒状体または線状体を溶接材料として用いて前記合金部材同士を溶接する溶接工程とを有することを特徴とする二相合金製造物の製造方法を提供するものである。
まず、本発明に係る二相合金の金属組織について説明する。
前述したように、本発明に係る二相合金は、Cr、NiおよびFeを主要成分とするCr-Ni-Fe系合金である。また、副成分として、MnおよびSiを少なくとも含み、追加的にV、Nb、TaおよびTiのうちの少なくとも一種を含み、更に不純物を含む。以下、本発明に係る二相合金の組成(各成分)について説明する。
Cr成分は、本二相合金の主要成分の1つであり、高強度のフェライト相を形成すると共に、オーステナイト相に固溶して耐食性の向上に寄与する成分である。Cr成分の含有率は、34質量%以上70質量%以下が好ましく、34質量%以上65質量%以下がより好ましく、40質量%以上60質量%以下が更に好ましい。Cr含有率が34質量%未満になると、フェライト率が10%未満(オーステナイト相の占有率が90%超)となり、二相合金の機械的強度が低下する。一方、Cr含有率が70質量%超になると、フェライト率が90%超(オーステナイト相の占有率が10%未満)となり、二相合金の延性・靱性が低下する。また、耐食性と材料コストとの観点から、主要3成分(Cr、Ni、Fe)のうちでCr成分が最大含有率であることが好ましい。
Ni成分は、本二相合金の主要成分の1つであり、オーステナイト相を安定化させて合金の二相状態の維持に寄与する(例えば、溶体化処理を施しても二相状態の維持が可能)と共に、二相合金に延性と靱性を付与する成分である。Ni成分の含有率は、17質量%以上45質量%以下が好ましく、20質量%以上40質量%以下がより好ましい。Ni含有率が17質量%未満になると、オーステナイト相の占有率が10%未満(フェライト率が90%超)となり、二相合金の延性・靱性が低下する。一方、Ni含有率が45質量%超になると、フェライト率が10%未満(オーステナイト相の占有率が90%超)となり、二相合金の機械的強度が低下する。
Fe成分も、本二相合金の主要成分の1つであり、機械的強度を確保するための基本成分である。Fe成分の含有率は、10質量%以上35質量%以下が好ましく、10質量%以上32質量%以下がより好ましい。Fe含有率が10質量%未満になると、二相合金の延性・靱性が低下する。一方、Fe含有率が35質量%超になると、800℃近傍の温度域で金属間化合物のσ相が生成し易くなり、二相合金の延性・靱性が著しく低下する(いわゆる、σ相脆化)。言い換えると、Feの含有率を10~35質量%の範囲に制御することにより、二相合金の機械的強度を確保しながらσ相の生成を抑制して延性・靱性の低下を抑制することができる。
Ni成分とFe成分との合計含有率は、30質量%以上65質量%以下が好ましく、40質量%以上62質量%以下がより好ましく、45質量%以上55質量%以下が更に好ましい。該合計含有率が30質量%未満になると、二相合金の延性・靱性が不十分になる。一方、該合計含有率が65質量%超になると、機械的強度が大きく低下する。
Mn成分は、本二相合金において脱硫・脱酸の役割を担い、機械的強度・靱性の向上および耐炭酸ガス腐食性の向上に寄与する副成分である。Mn成分の含有率は、0.1質量%以上2質量%以下が好ましく、0.3質量%以上1.8質量%以下がより好ましい。Mn含有率が0.1質量%未満になると、Mn成分による作用効果が十分に得られない。また、Mn含有率が2質量%超になると、硫化物(例えば、MnS)の粗大粒子を形成して耐食性や機械的強度の劣化要因になる。
Si成分は、本二相合金において脱酸の役割を担い、機械的強度・靱性の向上に寄与する副成分である。Si成分の含有率は、0.1質量%以上1質量%以下が好ましく、0.3質量%以上0.8質量%以下がより好ましい。Si含有率が0.1質量%未満になると、Si成分による作用効果が十分に得られない。また、Si含有率が1質量%超になると、酸化物(例えば、SiO2)の粗大粒子を形成して靱性の低下要因になる。
本二相合金における不純物としては、P、S、C、N、およびOが挙げられる。以下、それら不純物について説明する。
P成分は、二相合金の結晶粒界に偏析し易く、合金の靱性や粒界の耐食性を低下させる不純物成分である。P成分の含有率を0.04質量%以下に制御することで、それらの負の影響を抑制することができる。P含有率は、0.03質量%以下がより好ましい。
S成分は、本二相合金の構成成分と化合して比較的低融点の硫化物(例えば、Fe硫化物)を生成し易く、合金の靱性や耐孔食性を低下させる不純物成分である。S成分の含有率を0.01質量%以下に制御することで、それらの負の影響を抑制することができる。S含有率は、0.003質量%以下がより好ましい。
C成分は、固溶することによって合金を硬化させる作用効果がある一方、本二相合金の構成成分と化合して炭化物(例えば、Cr炭化物)を生成・粒界析出し易く、合金の耐食性や靱性を低下させる不純物成分でもある。C成分の含有率を0.03質量%以下に制御することで、それらの負の影響を抑制することができる。C含有率は、0.02質量%以下がより好ましい。
N成分は、固溶することによって合金を硬化させる作用効果がある一方、本二相合金の構成成分と化合して窒化物(例えば、Cr窒化物)を生成・析出し易く、合金の靱性を低下させる不純物成分でもある。N成分の含有率を0.02質量%以下に制御することで、その負の影響を抑制することができる。N含有率は、0.015質量%以下がより好ましい。
O成分は、本二相合金の構成成分と化合して酸化物(例えば、Fe酸化物)を生成・析出し易く、合金の靱性を低下させる不純物成分である。O成分の含有率を0.03質量%以下に制御することで、その負の影響を抑制することができる。O含有率は、0.02質量%以下がより好ましい。
本二相合金は、追加的副成分として、V、Nb、Ta、およびTiのうちの少なくとも一種を更に含むことが好ましい。以下、これら追加的副成分について説明する。
次に、上記の二相合金を用いた製造物、および該製造物の製造方法について説明する。図2は、本発明に係る二相合金製造物の製造方法の一例を示す工程図である。
次に、本発明の二相合金製造物およびその製造方法の他の実施形態について説明する。図3は、本発明に係る二相合金製造物の製造方法の他の一例を示す工程図である。図3の製造方法は、基材上に二相合金の被覆層を形成した複合体の製造方法の例であり、合金粉末を用いた積層造形について示した。
次に、本発明の二相合金製造物およびその製造方法の更に他の実施形態について説明する。図5は、本発明に係る二相合金製造物の製造方法の更に他の一例を示す工程図である。図5の製造方法は、本発明の二相合金からなる棒状材または線状材を作製し、該棒状材または線状材を溶接材料として用いて合金部材同士を溶接することについて示した。
表1に示す化学組成を有する発明合金1~8(IA 1~IA 8)および比較合金1~5(CA 1~CA 5)を用いて合金製造物(実施例1~14および比較例1~5)を作製した。なお、比較合金CA 5は、スーパー二相鋼と称される市販の二相ステンレス鋼である。各成分の含有率(単位:質量%)は、表1に記載の化学組成の総和が100質量%となるように換算してある。
(1)組織観察
各合金製造物から組織観察用の試験片を採取した後、該試験片の表面を鏡面研磨し、シュウ酸水溶液中で電界エッチングを行った。該研磨表面を光学顕微鏡で観察した。先に示した図1は、実施例5の金属組織の光学顕微鏡写真である。
組織観察用試験片の研磨表面に対して後方散乱電子回折像(EBSP)解析を行い、フェライト相の占有率(フェライト率、単位:%)を測定した。該測定には、株式会社日立ハイテクノロジーズ製の走査型電子顕微鏡(S-4300SE)に株式会社TSLソリューションズ製の結晶方位測定装置を付加した装置を用いた。結果を表2に併記する。
実施例の各合金製造物から組織安定性試験用の試験片を採取した後、800℃で60分間保持する熱処理を行った。各試験片の表面に対してX線回折測定を行い、金属間化合物のσ相の生成の有無を調査した。調査の結果、実施例1~14は、いずれもσ相が検出されず、σ相が生成し難いことが確認された。
機械的特性評価の一つとして、先の組織観察用試験片に対してビッカース硬度計を用いてビッカース硬さ試験(荷重:1 kg、荷重付加時間:15 s)を行った。ビッカース硬さは5測定の平均値として求めた。結果を表2に併記する。
用意した各合金製造物から引張試験用の試験片(直径:4 mm、平行部長さ:20 mm)を採取した。他の機械的特性評価として、各試験片に対して引張試験機を用いて室温引張試験(ひずみ速度:3×10-4 s-1)を行い、0.2%耐力、引張強さ、破断伸びを測定した。なお、明確な引張強さが測定される前に試験片が破断した場合は、破断応力を測定した。これら引張試験の結果は3測定の平均値として求めた。
耐食性評価の一種として孔食試験を行った。用意した各合金製造物から孔食試験用の分極試験片を採取した。孔食試験は、各分極試験片に対してJIS G0577(2005)に準拠して行った。具体的には、分極試験片にすきま腐食防止電極を装着し、参照電極として飽和カロメル電極を用い、分極試験片のアノード分極曲線を測定して、電流密度100μA/cm2に対応する孔食発生電位を求めた。孔食試験の結果を表2に併記する。また、アノード分極曲線測定後、光学顕微鏡を用いて孔食の発生の有無を調査した。
耐食性評価の他の一種として耐硫酸性試験を行った。孔食試験と同様に各合金製造物から耐硫酸性試験用の分極試験片を採取した。耐硫酸性試験は、具体的には、分極試験片にすきま腐食防止電極を装着し、硫酸水溶液(pH=2.0、30℃)中における分極試験片のアノード分極曲線(自然浸漬電位から掃引速度200μA/sの動電位法で電位1300 mV(vs. SHE)に達するまで)を測定した。得られた分極曲線から電位400 mV(vs. SHE)に対応する腐食電流密度を求めた。
表3に示す化学組成を有する発明合金9~17(IA 9~IA 17)を用いて合金製造物(実施例15~32)を作製した。なお、各成分の含有率(単位:質量%)は、表3に記載の化学組成の総和が100質量%となるように換算してある。
用意した実施例15~32に対して、先と同様に、組織観察、フェライト率測定、組織安定性試験、ビッカース硬さ試験、室温引張試験、孔食試験、および耐硫酸性試験を行った。それぞれの試験・評価結果を表4に示す。
表1に示した発明合金1~4(IA 1~IA 4)を用いて、図3に示した製造方法に沿って合金粉末(平均粒径100μm以下)を作製し、その後、金属粉末積層造形法により合金製造物(実施例33~36)を作製した。なお、本実験では、基材と複合していない成形体を造形した。
用意した実施例33~36に対して、先と同様に、組織観察、フェライト率測定、組織安定性試験、ビッカース硬さ試験、室温引張試験、および孔食試験を行い、実施例1,3,5,9と比較した。それぞれの製造方法と試験・評価結果とを後述する表5に示す。組織観察結果は、後述する図8a,図8bに示す。
Claims (20)
- Crを主要成分としフェライト相およびオーステナイト相の二相が混在する二相合金であって、
前記二相合金の化学組成は、
34質量%以上70質量%以下のCrと、
17質量%以上45質量%以下のNiと、
10質量%以上35質量%以下のFeと、
0.1質量%以上2質量%以下のMnと、
0.1質量%以上1質量%以下のSiと、
不純物とからなり、
前記Niと前記Feとの合計含有率が30質量%以上65質量%以下であることを特徴とする二相合金。 - 請求項1に記載の二相合金において、
前記不純物として、
0質量%超0.03質量%以下のCと、
0質量%超0.02質量%以下のNと、
0質量%超0.03質量%以下のOとを含み、
前記二相合金の構成成分として、V、Nb、TaおよびTiのうちの少なくとも一種を更に含み、
前記V、Nb、TaおよびTiの合計含有率が、前記C、NおよびOの合計含有率の0.8倍以上2倍以下の範囲であることを特徴とする二相合金。 - 請求項1又は請求項2に記載の二相合金において、
前記不純物として、
0質量%超0.04質量%以下のPと、
0質量%超0.01質量%以下のSとを含むことを特徴とする二相合金。 - 請求項1乃至請求項3のいずれか一項に記載の二相合金において、
前記フェライト相の占有率が10%以上90%以下であることを特徴とする二相合金。 - 二相合金を用いた製造物であって、
前記二相合金が、請求項1乃至請求項4のいずれか一項に記載の二相合金であることを特徴とする二相合金製造物。 - 請求項5に記載の二相合金製造物において、
前記製造物は、鍛造組織を有する成形体であることを特徴とする二相合金製造物。 - 請求項5に記載の二相合金製造物において、
前記製造物は、基材上に前記二相合金の被覆層が形成された複合体であることを特徴とする二相合金製造物。 - 請求項7に記載の二相合金製造物において、
前記被覆層中の前記フェライト相の平均Cr濃度に対する前記オーステナイト相の平均Cr濃度の比率が1.3以下であることを特徴とする二相合金製造物。 - 請求項7又は請求項8に記載の二相合金製造物において、
前記被覆層は、急冷凝固組織を有することを特徴とする二相合金製造物。 - 請求項6乃至請求項9のいずれか一項に記載の二相合金製造物において、
前記製造物は、回転機械の軸または軸受であることを特徴とする二相合金製造物。 - 請求項5に記載の二相合金製造物において、
前記製造物は、粉体であることを特徴とする二相合金製造物。 - 請求項5に記載の二相合金製造物において、
前記製造物は、棒状体または線状体であることを特徴とする二相合金製造物。 - 請求項11又は請求項12に記載の二相合金製造物において、
前記製造物は、溶接材料であることを特徴とする二相合金製造物。 - 請求項5に記載の二相合金製造物において、
前記製造物は、合金部材同士が溶接部を介して溶接された溶接継手であり、
前記溶接部が前記二相合金からなることを特徴とする二相合金製造物。 - 請求項14に記載の二相合金製造物において、
前記溶接部における前記フェライト相の平均Cr濃度に対する前記オーステナイト相の平均Cr濃度の比率が1.3以下であることを特徴とする二相合金製造物。 - 請求項14又は請求項15に記載の二相合金製造物において、
前記合金部材が前記二相合金からなることを特徴とする二相合金製造物。 - 請求項5又は請求項6に記載の二相合金製造物の製造方法であって、
前記二相合金の原料を混合・溶解する原料混合溶解工程と、
鋳造して鋳塊を形成する鋳造工程と、
前記鋳塊を熱間鍛造して成形体を形成する熱間鍛造成形工程と、
前記成形体に対して1050℃以上1250℃以下の温度範囲で溶体化処理を施す溶体化熱処理工程とを有することを特徴とする二相合金製造物の製造方法。 - 請求項17に記載の二相合金製造物の製造方法において、
前記溶体化熱処理工程の後に、溶体化処理した前記成形体に対して800℃以上1000℃以下の温度範囲で時効処理を施す時効熱処理工程を更に有することを特徴とする二相合金製造物の製造方法。 - 請求項7乃至請求項9のいずれか一項に記載の二相合金製造物の製造方法であって、
前記二相合金の原料を混合・溶解して溶湯を形成する原料混合溶解工程と、
前記溶湯から合金粉末を形成するアトマイズ工程と、
前記合金粉末を用いて前記基材上に前記二相合金の被覆層を形成する積層造形工程とを有することを特徴とする二相合金製造物の製造方法。 - 請求項14乃至請求項16のいずれか一項に記載の二相合金製造物の製造方法であって、
前記二相合金の原料を混合・溶解する原料混合溶解工程と、
鋳造して鋳塊を形成する鋳造工程と、
前記鋳塊を熱間加工して棒状体または線状体を形成する熱間加工成形工程と、
前記棒状体または線状体を溶接材料として用いて前記合金部材同士を溶接する溶接工程とを有することを特徴とする二相合金製造物の製造方法。
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US (1) | US10718038B2 (ja) |
EP (1) | EP3202934B1 (ja) |
JP (1) | JP6374520B2 (ja) |
WO (1) | WO2016052445A1 (ja) |
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WO2017168640A1 (ja) * | 2016-03-30 | 2017-10-05 | 株式会社日立製作所 | クロム基二相合金製造物およびその製造方法 |
WO2017168806A1 (ja) * | 2016-03-30 | 2017-10-05 | 株式会社日立製作所 | クロム基二相合金製造物およびその製造方法 |
WO2018066303A1 (ja) * | 2016-10-03 | 2018-04-12 | 株式会社日立製作所 | Cr基二相合金製造物およびその製造方法 |
WO2018186298A1 (ja) * | 2017-04-03 | 2018-10-11 | 日立金属株式会社 | Cr-Fe-Ni系合金製造物およびその製造方法 |
WO2019064641A1 (ja) * | 2017-09-28 | 2019-04-04 | 株式会社日立製作所 | 合金部材及びそれを用いた製造物 |
JP2019065389A (ja) * | 2017-09-29 | 2019-04-25 | 日立金属株式会社 | Cr−Fe−Ni系合金製造物及びその製造方法 |
JP2019143192A (ja) * | 2018-02-20 | 2019-08-29 | 株式会社日立製作所 | Cr−Fe−Ni系合金製造物 |
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EP3441492A4 (en) * | 2016-03-30 | 2019-09-25 | Hitachi, Ltd. | TWO-PHASE CHROMIUM-BASED ALLOY AND PRODUCT USING SAID TWO PHASE ALLOY |
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Also Published As
Publication number | Publication date |
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JPWO2016052445A1 (ja) | 2017-04-27 |
EP3202934A1 (en) | 2017-08-09 |
EP3202934A4 (en) | 2018-05-02 |
US20170292175A1 (en) | 2017-10-12 |
US10718038B2 (en) | 2020-07-21 |
JP6374520B2 (ja) | 2018-08-15 |
EP3202934B1 (en) | 2019-07-24 |
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