WO2020179207A1 - コバルト基合金粉末、コバルト基合金焼結体およびコバルト基合金焼結体の製造方法 - Google Patents
コバルト基合金粉末、コバルト基合金焼結体およびコバルト基合金焼結体の製造方法 Download PDFInfo
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- F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
- F01D5/12—Blades
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- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/08—Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
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- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/009—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine components other than turbine blades
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/04—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine blades
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
- F05D2230/00—Manufacture
- F05D2230/20—Manufacture essentially without removing material
- F05D2230/22—Manufacture essentially without removing material by sintering
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
- F05D2300/00—Materials; Properties thereof
- F05D2300/10—Metals, alloys or intermetallic compounds
- F05D2300/17—Alloys
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- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
Definitions
- the present invention relates to a cobalt-based alloy powder, a cobalt-based alloy sintered body, and a method for producing a cobalt-based alloy sintered body.
- Co-based alloy materials are typical heat-resistant alloy materials together with nickel (Ni)-based alloy materials, and are also called superalloys and widely used for high-temperature members of turbines (for example, gas turbines and steam turbines). There is.
- the Co-based alloy material has a higher material cost than the Ni-based alloy material, but has excellent corrosion resistance and wear resistance and is easily solid-solution strengthened, and thus has been used as a turbine vane or a combustor member.
- the Ni-based alloy material is strengthened by the precipitation of the ⁇ 'phase (for example, Ni 3 (Al, Ti) phase). It was developed and is now mainstream.
- the Co-based alloy material since it is difficult to precipitate an intermetallic compound phase such as the ⁇ 'phase of the Ni-based alloy material, which greatly contributes to the improvement of mechanical properties, precipitation strengthening by the carbide phase has been studied.
- Patent Document 1 Japanese Patent Laid-Open No. 61-243143
- massive and granular carbides having a grain size of 0.5 to 10 ⁇ m are deposited on a base of a cobalt-based alloy having a grain size of 10 ⁇ m or less.
- a Co-based superplastic alloy is disclosed.
- the cobalt-based alloy has a weight ratio of C: 0.15 to 1%, Cr: 15 to 40%, W and/or Mo: 3 to 15%, B: 1% or less, Ni: 0 to 20%,
- Nb 0 to 1.0%
- Zr 0 to 1.0%
- Ta 0 to 1.0%
- Ti 0 to 3%
- Al 0 to 3%
- the balance Co is that
- a Co-based superplastic material that exhibits superplasticity even in a low temperature region (for example, 950° C.), has an elongation of 70% or more, and can produce a complex-shaped object by plastic working such as forging. It is said that it can provide alloys.
- Patent Document 2 Japanese Unexamined Patent Publication No. 7-179967
- Cr 21 to 29%
- Mo 15 to 24%
- B 0.5 to 2%
- Si 0.1% or more are 0 in weight%.
- the Co-based alloy has a composite structure in which molybdenum boride and chromium carbide are relatively finely dispersed in a quaternary alloy phase of Co, Cr, Mo, and Si, and has good corrosion resistance and resistance. It is said to have wear resistance and high strength.
- the Co-based alloy materials described in Patent Documents 1 and 2 are considered to have higher mechanical properties than the Co-based alloy materials before them, but compared with the recent precipitation strengthened Ni-based alloy materials. However, it cannot be said that it has sufficient mechanical properties. However, if it is possible to achieve mechanical properties equivalent to or higher than those of the ⁇ 'phase precipitation strengthened Ni-based alloy material (for example, a creep durability temperature of 100,000 hours at 58 MPa is 875° C. or higher, and a tensile strength at room temperature is 500 MPa or higher),
- the Co-based alloy material can be a material suitable for a turbine high temperature member.
- the present invention has been made in view of the above problems, and an object thereof is a Co-based alloy powder capable of providing a Co-based alloy material having mechanical properties equal to or higher than that of a precipitation strengthened Ni-based alloy material, It is to provide a Co-based alloy sintered body and a method for manufacturing a Co-based alloy sintered body.
- One aspect of the cobalt-based alloy powder of the present invention for achieving the above object is 0.08% by mass or more and 0.25% by mass or less of carbon, Boron of 0.1% by mass or less and 10 mass% or more and 30 mass% or less of chromium, Iron of 5% by mass or less and Including 30% by mass or less of nickel, Contains iron and nickel so that the total is 30% by mass or less.
- At least one of tungsten and molybdenum is included so that the total amount is 5% by mass or more and 12% by mass or less
- At least one of titanium, zirconium, niobium, tantalum, hafnium, and vanadium is contained so that the total is 0.5% by mass or more and 2% by mass or less
- With 0.5% by mass or less of silicon, With 0.5% by mass or less of manganese It contains 0.003% by mass or more and 0.04% by mass or less of nitrogen, the balance consisting of cobalt and impurities, the crystal grains constituting the cobalt-based alloy powder have segregation cells, and the average size of the segregation cells is 0. It is characterized in that it is not less than 0.15 ⁇ m and not more than 4 ⁇ m.
- one aspect of the cobalt-based alloy sintered body of the present invention for achieving the above object is. 0.08% by mass or more and 0.25% by mass or less of carbon, Boron of 0.1% by mass or less and 10 mass% or more and 30 mass% or less of chromium, Iron of 5% by mass or less and Including 30% by mass or less of nickel, Contains iron and nickel so that the total is 30% by mass or less.
- At least one of tungsten and molybdenum is included so that the total amount is 5% by mass or more and 12% by mass or less
- At least one of titanium, zirconium, niobium, tantalum, hafnium, and vanadium is contained so that the total is 0.5% by mass or more and 2% by mass or less
- With 0.5% by mass or less of silicon, With 0.5% by mass or less of manganese The content of nitrogen is 0.04 mass% or more and 0.1 mass% or less, and the balance is cobalt and impurities. Is 0.15 ⁇ m or more and 4 ⁇ m or less.
- one aspect of the method for producing a cobalt-based alloy sintered body of the present invention for achieving the above object is to mix raw materials of the cobalt-based alloy powder having the above-described chemical composition and melt them to prepare a molten metal.
- the cobalt-based alloy powder of the present invention is the above-mentioned cobalt-based alloy powder having a melting step, a melt-powdering step of forming a rapidly solidified alloy powder from the molten metal, and a sintering step of sintering the rapidly solidified alloy powder. It is characterized by having the composition of.
- a Co-based alloy powder, a Co-based alloy sintered body, and a method for producing a Co-based alloy sintered body capable of providing a Co-based alloy material having mechanical properties equal to or higher than those of a precipitation strengthened Ni-based alloy material Can be provided.
- the final solidified parts eg dendrite boundaries and crystal grains
- the boundary has the property of being significantly segregated. Therefore, in the conventional Co-based alloy material, the carbide phase particles are precipitated along the dendrite boundaries or the crystal grain boundaries of the matrix phase.
- the average interval and the average crystal grain size of the dendrite boundaries is 10 1 ⁇ 10 2 ⁇ m order, the average spacing of the carbide phase particles to 10 1 ⁇ 10 2 ⁇ m order Become. Even in a process such as laser welding in which the solidification rate is relatively fast, the average interval of the carbide phase particles in the solidified portion is about 5 ⁇ m.
- the precipitation strengthening in an alloy is inversely proportional to the average spacing between the precipitates, and it is said that the precipitation strengthening becomes effective when the average spacing between the precipitates is about 2 ⁇ m or less.
- the average spacing between the precipitates does not reach that level, and the effect of sufficient precipitation strengthening cannot be obtained.
- Cr carbide phase is another carbide phase that can be precipitated in a Co-based alloy. Since the Cr component has a high solid solubility in the Co-based alloy parent phase and is difficult to segregate, the Cr carbide phase can be dispersed and precipitated in the parent phase crystal grains. However, it is known that the Cr carbide phase has low lattice consistency with the Co-based alloy matrix crystal and is not so effective as a precipitation strengthening phase.
- the present inventors can dramatically improve the mechanical properties of the Co-based alloy material if the carbide phase particles contributing to precipitation strengthening can be dispersed and precipitated in the matrix crystal grains. I thought I could do it. Further, it was thought that a heat-resistant alloy material superior to the precipitation-strengthened Ni-based alloy material could be provided in combination with the good corrosion resistance and wear resistance originally possessed by the Co-based alloy material.
- the present inventors have diligently studied the alloy composition and the manufacturing method for obtaining such a Co-based alloy material. As a result, they have found that by optimizing the alloy composition, carbide phase particles that contribute to alloy strengthening can be dispersed and precipitated in the matrix crystal grains of the Co-based alloy material. The present invention has been completed based on this finding.
- the C component is referred to as an MC-type carbide phase (Ti, Zr, Nb, Ta, Hf and / or V carbide phase or enhanced carbide phase) which is a precipitation strengthening phase. In some cases) is an important ingredient that constitutes.
- the content of the C component is preferably 0.08 mass% or more and 0.25 mass% or less, more preferably 0.1 mass% or more and 0.2 mass% or less, and 0.12 mass% or more and 0.18 mass% or less. Is more preferable.
- the C content is less than 0.08% by mass, the amount of the strengthened carbide phase precipitated is insufficient, and the effect of improving the mechanical properties cannot be sufficiently obtained.
- the C content exceeds 0.25% by mass, excessive hardening causes the ductility and toughness of the sintered body obtained by sintering the Co-based alloy to decrease.
- the B component is a component that contributes to the improvement of the bondability of the crystal grain boundaries (so-called grain boundary strengthening).
- grain boundary strengthening a component that contributes to the improvement of the bondability of the crystal grain boundaries.
- the component B is not an essential component, when it is contained, it is preferably 0.1 mass% or less, more preferably 0.005 mass% or more and 0.05 mass% or less. If the B content exceeds 0.1% by mass, cracks are likely to occur during sintering of the Co-based alloy and subsequent heat treatment.
- the Cr component is a component that contributes to the improvement of corrosion resistance and oxidation resistance.
- the content of the Cr component is preferably 10% by mass or more and 30% by mass or less, and more preferably 10% by mass or more and 25% by mass or less.
- the content of the Cr component is more preferably 10% by mass or more and 18% by mass or less. If the Cr content is less than 10% by mass, corrosion resistance and oxidation resistance will be insufficient. On the other hand, when the Cr content exceeds 30% by mass, a brittle ⁇ phase or a Cr carbide phase is formed, and the mechanical properties (toughness, ductility, strength) are lowered.
- Ni 30% by mass or less Since the Ni component has similar characteristics to the Co component and is cheaper than Co, it is a component that can be contained by partially replacing the Co component.
- the Ni component is not an essential component, but when it is contained, it is preferably 30% by mass or less, more preferably 20% by mass or less, and further preferably 5% by mass or more and 15% by mass or less.
- the Ni content exceeds 30% by mass, the wear resistance and the resistance to local stress, which are the characteristics of Co-based alloys, deteriorate. This is considered to be due to the difference between the stacking defect energy of Co and that of Ni.
- the Fe component is much cheaper than Ni and has properties similar to those of the Ni component, so that the Fe component can be contained in a form that replaces a part of the Ni component. That is, the total content of Fe and Ni is preferably 30% by mass or less, more preferably 20% by mass or less, and further preferably 5% by mass or more and 15% by mass or less.
- the Fe component is not an essential component, but when it is contained, it is preferably 5% by mass or less and more preferably 3% by mass or less within a range smaller than the Ni content. When the Fe content exceeds 5 mass %, it becomes a cause of deterioration of corrosion resistance and mechanical properties.
- W and / or Mo Total 5% by mass or more and 12% by mass or less
- the W component and the Mo component are components that contribute to the solid solution strengthening of the matrix.
- the total content of the W component and / or the Mo component is preferably 5% by mass or more and 12% by mass or less, and more preferably 7% by mass or more and 10% by mass or less. If the total content of the W component and the Mo component is less than 5% by mass, solid solution strengthening of the parent phase becomes insufficient. On the other hand, when the total content of the W component and the Mo component exceeds 12% by mass, a brittle ⁇ phase is likely to be generated and mechanical properties (toughness, ductility) are deteriorated.
- the Re component is a component that contributes to solid solution strengthening of the mother phase and contributes to improvement of corrosion resistance.
- the Re component is not an essential component, but when it is contained, it is preferably 2% by mass or less, more preferably 0.5% by mass or more and 1.5% by mass or less in the form of partially replacing the W component or Mo component. If the Re content exceeds 2% by mass, not only the action and effect of the Re component are saturated, but also the material cost increases, which is a demerit.
- Ti, Zr, Nb, Ta, Hf and V 0.5% by mass or more and 2% by mass or less in total Ti component, Zr component, Nb component, Ta component, Hf component and V component are reinforced carbide phases ( It is an important component that constitutes the MC type carbide phase).
- the total content of one or more of Ti, Zr, Nb, Ta, Hf and V components is preferably 0.5% by mass or more and 2% by mass or less, and more preferably 0.5% by mass or more and 1.8% by mass or less. preferable. If the total content is less than 0.5% by mass, the amount of the reinforced carbide phase precipitated is insufficient, and the effect of improving the mechanical properties cannot be sufficiently obtained.
- the strengthened carbide phase particles are coarsened, the formation of brittle phase (for example, ⁇ phase) is promoted, and oxide phase particles that do not contribute to precipitation strengthening are generated. The mechanical properties are reduced.
- the content when Ti is contained is preferably 0.01% by mass or more and 1% by mass or less, and more preferably 0.05% by mass or more and 0.8% by mass or less.
- Zr is contained
- the content is preferably 0.05% by mass or more and 1.5% by mass or less, and more preferably 0.1% by mass or more and 1.2% by mass or less.
- Nb is contained
- the content is preferably 0.02% by mass or more and 1% by mass or less, and more preferably 0.05% by mass or more and 0.8% by mass or less.
- Ta is contained, the content is preferably 0.05% by mass or more and 1.5% by mass or less, and more preferably 0.1% by mass or more and 1.2% by mass or less.
- the content is preferably 0.01% by mass or more and 0.5% by mass or less, and more preferably 0.02% by mass or more and 0.1% by mass or less.
- V is contained, the content is preferably 0.01% by mass or more and 0.5% by mass or less, and more preferably 0.02% by mass or more and 0.1% by mass or less.
- the Si component plays a role of deoxidation and contributes to the improvement of mechanical properties.
- the Si component is not an essential component, but when contained, it is preferably 0.5 mass% or less, more preferably 0.01 mass% or more and 0.3 mass% or less. If the Si content exceeds 0.5% by mass, coarse particles of an oxide (for example, SiO 2 ) are formed, which causes deterioration of mechanical properties.
- the Mn component is a component that plays a role of deoxidation and desulfurization and contributes to improvement of mechanical properties and corrosion resistance.
- the Mn component is not an essential component, when it is contained, it is preferably 0.5 mass% or less, more preferably 0.01 mass% or more and 0.3 mass% or less.
- MnS coarse particles of sulfide
- N 0.003% by mass or more and 0.04% by mass or less or more than 0.04% by mass and 0.1% by mass or less
- the content of the N component varies depending on the gas atomizing atmosphere when the Co-based alloy powder is manufactured.
- the content of the N component becomes low (N: 0.003 mass% or more and 0.04 mass% or less)
- N The content of the component becomes high (N: 0.04 mass% or more and 0.1 mass% or less).
- the N component is a component that contributes to the stable formation of a strengthened carbide phase. If the N content is less than 0.003% by mass, the action and effect of the N component cannot be sufficiently obtained. On the other hand, if the N content exceeds 0.1% by mass, coarse particles of nitride (for example, Cr nitride) are formed, which causes deterioration of mechanical properties.
- nitride for example, Cr nitride
- Co component+impurity The Co component is one of the main components of the present alloy, and is the component with the maximum content. As described above, the Co-based alloy material has an advantage that it has corrosion resistance and wear resistance equal to or higher than that of the Ni-based alloy material.
- the Al component is one of the impurities of the present alloy and is not a component intentionally included. However, an Al content of 0.5 mass% or less is acceptable because it does not have a large adverse effect on the mechanical properties of the Co-based alloy product. If the Al content exceeds 0.5 mass %, coarse particles of oxides or nitrides (for example, Al 2 O 3 or AlN) are formed, which causes a decrease in mechanical properties.
- the O component is also one of the impurities in this alloy and is not a component that is intentionally included. However, an O content of 0.04% by mass or less is acceptable because it does not significantly adversely affect the mechanical properties of the Co-based alloy product. If the O content exceeds 0.04% by mass, coarse particles of various oxides (for example, Ti oxide, Zr oxide, Al oxide, Fe oxide, Si oxide) are formed to improve mechanical properties. It becomes a decrease factor.
- various oxides for example, Ti oxide, Zr oxide, Al oxide, Fe oxide, Si oxide
- FIG. 2 is a flow chart showing an example of steps of a method for producing a Co-based alloy powder and a Co-based alloy sintered body according to the present invention.
- a raw material mixing and dissolving step step 1: of mixing and melting the raw materials of the Co-based alloy powder to form the molten metal 10 so as to have the composition of the Co-based alloy powder of the present invention described above.
- the melting method is not particularly limited, and the conventional method for the high heat resistant alloy (for example, the induction melting method, the electron beam melting method, the plasma arc melting method) can be preferably used.
- the molten metal 10 is formed and then once solidified to form a raw material alloy ingot, and thereafter, It is preferable to remelt the raw alloy ingot to form a cleansing melt.
- the remelting method is not particularly limited as long as the cleanliness of the alloy can be improved, but for example, the vacuum arc remelting (VAR) method can be preferably used.
- a melt-powdering step (step 2: S2) of forming the rapidly solidified Co-based alloy powder 20 from the melt 10 (or the cleaned melt) is performed. Since the Co-based alloy powder of the present invention is produced by rapid solidification with a high cooling rate, it is possible to obtain a segregation cell as shown in FIG. 1, which improves the strength of the Co-based alloy product. The average size of the segregation cell decreases as the cooling rate increases.
- melt-powderization method there is no particular limitation on the melt-powderization method as long as a highly clean and homogeneous composition can be obtained, and the conventional alloy powder manufacturing method (for example, atomizing method (gas atomizing method, plasma atomizing method), water atomizing method) can be preferably used.
- atomizing method gas atomizing method, plasma atomizing method
- water atomizing method water atomizing method
- FIG. 1 is a diagram schematically showing the powder surface of the Co-based alloy powder of the present invention.
- the Co-based alloy powder 20 of the present invention is a polycrystalline body composed of a powder 21 having an average powder particle size of 5 ⁇ m or more and 150 ⁇ m or less, and a segregation cell is formed on the surface and inside of the powder 21. 22 is formed.
- the segregation cell 22 changes its shape depending on the cooling rate in the step of producing Co-based alloy powder (powderizing step) described later.
- FIG. 1 shows an example in which the segregation cells are dendrite-shaped (dendritic). It is considered that after sintering the Co-based alloy powder 20, carbide is deposited along this segregation cell.
- the average size of the segregation cell is preferably 0.15 ⁇ m or more and 4 ⁇ m or less.
- the dendrite structure 22 shown in FIG. 1 has a primary branch 24 extending along the coagulation direction and a secondary branch 25 extending from the primary branch 24.
- the average size of the segregation cells in the dendrite structure is the average width (arm interval) 23 of this secondary branch 25 (the portion shown by the arrow in FIG. 1).
- the “average size of the segregation cell” shall indicate the diameter.
- the “average size of the segregation cell” is a value obtained by averaging the sizes of the segregation cells in a predetermined area of an observation image such as SEM (Scanning Electron Microscope).
- the Co-based alloy powder of the present invention preferably has a particle size of 5 ⁇ m or more and 85 ⁇ m or less. It is more preferably 10 ⁇ m or more and 85 ⁇ m or less, and further preferably 5 ⁇ m or more and 25 ⁇ m or less.
- the preferable composition of the Co-based alloy powder of the present invention is shown in Table 1 below.
- the Co-based alloy sintered body of the present invention can be obtained by performing the sintering step (Step 3: S3) of sintering the Co-based alloy powder 20 generated by rapid solidification.
- the sintering method is not particularly limited, and for example, a hot isostatic pressing (Hot Isostatic Pressing) can be used.
- a molded body (diameter 8 mm ⁇ height 10 mm) was formed by HIP using the alloy powders of grain size S of IA-2 and CA-5 in Table 1.
- the HIP sintering conditions were 1150° C., 150 MPa, and 1 hour.
- heat treatment was carried out at 980 ° C. for 4 hours to prepare a sintered body using IA-2 powder and a sintered body using CA-5 powder.
- a cast body (diameter 8 mm x height 10 mm) is formed by a precision casting method using the above-mentioned alloy powder having a particle size of L of IA-2 and CA-5, and the same solution heat treatment step and aging heat treatment step as described above are performed. Then, a cast alloy product (cast body) using IA-2 powder and a cast alloy product (cast body) using CA-5 powder were prepared.
- Microstructure observation and mechanical property test From the sintered body and the cast body produced as described above, test pieces for microstructure observation and mechanical property test were respectively collected, and microstructure observation and mechanical property test were performed.
- Microstructure observation was performed by SEM. Further, the obtained SEM observation image was subjected to image analysis using image processing software (public domain software developed by ImageJ, National Institutes of Health (NIH)), and the average size of the segregation cells, the average interval of microsegregation, and The average interparticle distance of the carbide phase particles was measured.
- image processing software public domain software developed by ImageJ, National Institutes of Health (NIH)
- FIG. 5 is an SEM observation photograph of the Co-based alloy sintered body of the present invention.
- FIG. 5 shows SEMs of Co-based alloy powders having three types of particle sizes (5 to 25 ⁇ m, 10 to 85 ⁇ m, and 70 ⁇ m or more) that have been heat-treated (982 ° C., 4 hours) immediately after HIP and after HIP. It is a photograph which was observed in (Scanning Electron Microscope). It can be seen that the structure of the sintered body is maintained before and after the heat treatment. Further, the sintered body using the powder having any particle size had a fine structure in which the reinforced carbide phase particles were precipitated. It is considered that the reinforced carbide phase particles were precipitated along the segregation cell of the Co-based alloy powder by sintering.
- Table 2 shows the 0.2% proof stress and tensile strength of the Co-based alloy sintered body of the present invention
- Table 3 shows the average precipitate interval L and the tensile strength of the Co-based alloy sintered body.
- Table 2 also shows the results for the cast material. As shown in Table 2, each particle size achieves 0.2% proof stress and tensile strength higher than those of the cast material. Further, it can be seen from Table 3 that particularly high tensile strength (460 MPa or more) is achieved when the average precipitate spacing L is 1 to 1.49 ⁇ m.
- FIG. 6 is a graph showing the relationship between the average size of the segregation cells in the Co-based alloy sintered body and the cast body and the 0.2% proof stress at 800° C. Note that FIG. 6 also shows the data of the cast body as a comparison. In the cast, the average size of the segregation cells was substituted by the average interval of microsegregation.
- "IA-2" and "CA-5" are Co-based alloy powders having the compositions shown in Table 1.
- the Co-based alloy sintered body prepared using CA-5 powder showed an almost constant 0.2% proof stress without being affected by the average size of the segregated cells.
- the yield strength of the Co-based alloy sintered body prepared using the IA-2 powder changed significantly by 0.2% depending on the average size of the segregated cells.
- CA-5 powder has an excessively low total content of “Ti+Zr+Nb+Ta+Hf+V” (almost not included). Therefore, as a result of observing the structure, the sintered body using the CA-5 powder had a fine structure in which the reinforced carbide phase was not precipitated but Cr carbide particles were precipitated. This result confirms that the Cr carbide particles are not very effective as precipitation strengthening particles. On the other hand, the sintered body using the IA-2 powder had a fine structure in which reinforced carbide phase particles were precipitated. Therefore, it is considered that the 0.2% proof stress changed significantly depending on the average size of the segregated cells (the resulting average interparticle distance of the carbide phase particles).
- the 0.2% proof stress at 800 ° C. is required to be 250 MPa or more. Therefore, if 0.2% proof stress of more than 250 MPa is judged as “pass” and less than 250 MPa is judged as “fail”, the average size of the segregation cell (the resulting average inter-particle distance of the carbide phase particles) is 0. It was confirmed that mechanical properties of “pass” were obtained in the range of 0.15 to 4 ⁇ m. In other words, it is considered that one of the factors that the conventional carbide phase precipitation Co-based alloy material could not obtain sufficient mechanical properties is that the average interparticle distance of the reinforced carbide phase particles could not be controlled within a desired range.
- the heat treatment causes the carbides on the segregation cells to agglomerate and the inter-particle distance of the carbide phase particles to expand, resulting in a decrease in 0.2% proof stress. Further, even if it exceeds 4 ⁇ m, the influence on the 0.2% proof stress becomes small.
- the average size of the segregation cells constituting the Co-based alloy powder of the present invention is also preferably 0.15 to 4 ⁇ m.
- the average size of the segregation cell is more preferably 0.15 to 2 ⁇ m, further preferably 0.15 to 1.5 ⁇ m.
- the average size of the segregation cells is about the same as the average size of the segregation cells of the Co alloy powder by appropriate sintering. It is considered that a Co-based alloy powder sintered body in which carbides are precipitated at intervals of 15 to 4 ⁇ m can be obtained.
- the raw material of the Co-based alloy sintered body of the present invention preferably contains 75% by mass or more, and more preferably 90% by mass or more of the above Co-based alloy powder.
- FIG. 3 is an example of a Co-based alloy product of the present invention, and is a schematic perspective view showing a turbine vane as a turbine high temperature member.
- the turbine stationary blade 100 is roughly composed of an inner ring side end wall 101, a blade portion 102, and an outer ring side end wall 103. Cooling structures are often formed inside the wings. Note that, for example, in the case of a power generation gas turbine with an output of 30 MW, the length of the blade portion of the turbine vane (distance between both end walls) is about 170 mm.
- FIG. 4 is a schematic cross-sectional view showing an example of a gas turbine equipped with the Co-based alloy product according to the present invention.
- the gas turbine 200 is roughly configured by a compressor unit 210 that compresses intake air and a turbine unit 220 that blows combustion gas of fuel to turbine blades to obtain rotational power.
- the turbine high temperature member of the present invention can be suitably used as a turbine nozzle 221 or a turbine stationary blade 100 in the turbine section 220.
- the turbine high temperature member of the present invention is not limited to gas turbine applications, and may be used for other turbine applications (for example, steam turbine applications).
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Abstract
Description
性及び耐摩耗性、並びに高い強度を備える、とされている。
0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
鉄とニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.003質量%以上0.04質量%以下の窒素とを含み、残部がコバルトと不純物とからなり、コバルト基合金粉末を構成する結晶粒が偏析セルを有し、偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とする。
0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
鉄とニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.04質量%以上0.1質量%以下の窒素とを含み、残部がコバルトと不純物とからなり、なり、コバルト基合金粉末を構成する結晶粒が偏析セルを有し、偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とする。
前述したように、Co基合金材では、炭化物相の析出による強化が種々研究開発されてきた。析出強化に寄与する炭化物相としては、例えば、Ti、Zr、Nb、Ta、HfおよびVのMC型炭化物相(Mは遷移金属を意味し、Cは炭素を意味する。)、およびそれら金属元素の複合炭化物相が挙げられる。
上述した本発明のCo基合金粉末の化学組成について、以下に説明する。
C成分は、析出強化相となるMC型炭化物相(Ti、Zr、Nb、Ta、Hfおよび/またはVの炭化物相、強化炭化物相と称する場合がある)を構成する重要な成分である。C成分の含有率は、0.08質量%以上0.25質量%以下が好ましく、0.1質量%以上0.2質量%以下がより好ましく、0.12質量%以上0.18質量%以下が更に好ましい。C含有率が0.08質量%未満になると、強化炭化物相の析出量が不足し、機械的特性向上の作用効果が十分に得られない。一方、C含有率が0.25質量%超になると、過度に硬化することで、Co基合金を焼結して得た焼結体の延性や靭性が低下する。
B成分は、結晶粒界の接合性の向上(いわゆる粒界強化)に寄与する成分である。B成分は必須成分ではないが、含有させる場合、0.1質量%以下が好ましく、0.005質量%以上0.05質量%以下がより好ましい。B含有率が0.1質量%超になると、Co基合金の焼結時やその後の熱処理で割れが発生し易くなる。
Cr成分は、耐食性や耐酸化性の向上に寄与する成分である。Cr成分の含有率は、10質量%以上30質量%以下が好ましく、10質量%以上25質量%以下がより好ましい。Co基合金製造物の最表面に耐食性被覆層を別途設けるような場合は、Cr成分の含有率は、10質量%以上18質量%以下が更に好ましい。Cr含有率が10質量%未満になると、耐食性や耐酸化性が不十分になる。一方、Cr含有率が30質量%超になると、脆性のσ相が生成したりCr炭化物相が生成したりして機械的特性(靱性、延性、強さ)が低下する。
Ni成分は、Co成分と類似した特性を有しかつCoに比して安価なことから、Co成分の一部を置き換えるかたちで含有させることができる成分である。Ni成分は必須成分ではないが、含有させる場合、30質量%以下が好ましく、20質量%以下がより好ましく、5質量%以上15質量%以下が更に好ましい。Ni含有率が30質量%超になると、Co基合金の特徴である耐摩耗性や局所応力への耐性が低下する。これは、Coの積層欠陥エネルギーとNiのそれとの差異に起因すると考えられる。
Fe成分は、Niよりもはるかに安価でありかつNi成分と類似した性状を有することから、Ni成分の一部を置き換えるかたちで含有させることができる成分である。すなわち、FeおよびNiの合計含有率は30質量%以下が好ましく、20質量%以下がより好ましく、5質量%以上15質量%以下が更に好ましい。Fe成分は必須成分ではないが、含有させる場合、Ni含有率よりも少ない範囲で5質量%以下が好ましく、3質量%以下がより好ましい。Fe含有率が5質量%超になると、耐食性や機械的特性の低下要因になる。
W成分およびMo成分は、母相の固溶強化に寄与する成分である。W成分および/またはMo成分の含有率は、合計で5質量%以上12質量%以下が好ましく、7質量%以上10質量%以下がより好ましい。W成分とMo成分との合計含有率が5質量%未満になると、母相の固溶強化が不十分になる。一方、W成分とMo成分との合計含有率が12質量%超になると、脆性のσ相が生成し易くなって機械的特性(靱性、延性)が低下する。
Re成分は、母相の固溶強化に寄与すると共に、耐食性の向上に寄与する成分である。Re成分は必須成分ではないが、含有させる場合、W成分またはMo成分の一部を置き換えるかたちで2質量%以下が好ましく、0.5質量%以上1.5質量%以下がより好ましい。Re含有率が2質量%超になると、Re成分の作用効果が飽和するのに加えて、材料コストの増加がデメリットになる。
Ti成分、Zr成分、Nb成分、Ta成分、Hf成分およびV成分は、強化炭化物相(MC型炭化物相)を構成する重要な成分である。Ti、Zr、Nb、Ta、HfおよびV成分の1種以上の合計含有率は、0.5質量%以上2質量%以下が好ましく、合計0.5質量%以上1.8質量%以下がより好ましい。合計含有率が0.5質量%未満になると、強化炭化物相の析出量が不足し、機械的特性向上の作用効果が十分に得られない。一方、当該合計含有率が2質量%超になると、強化炭化物相粒子が粗大化したり脆性相(例えばσ相)の生成を促進したり析出強化に寄与しない酸化物相粒子を生成したりして機械的特性が低下する。
Si成分は、脱酸素の役割を担って機械的特性の向上に寄与する成分である。Si成分は必須成分ではないが、含有させる場合、0.5質量%以下が好ましく、0.01質量%以上0.3質量%以下がより好ましい。Si含有率が0.5質量%超になると、酸化物(例えばSiO2)の粗大粒子を形成して機械的特性の低下要因になる。
Mn成分は、脱酸素・脱硫の役割を担って機械的特性の向上や耐腐食性の向上に寄与する成分である。Mn成分は必須成分ではないが、含有させる場合、0.5質量%以下が好ましく、0.01質量%以上0.3質量%以下がより好ましい。Mn含有率が0.5質量%超になると、硫化物(例えばMnS)の粗大粒子を形成して機械的特性や耐食性の低下要因になる。
N成分は、Co基合金粉末を製造する際のガスアトマイズの雰囲気によって含有量が異なる。ガスアトマイズをアルゴンガス雰囲気中で行った場合にはN成分の含有量は低くなり(N:0.003質量%以上0.04質量%以下)、ガスアトマイズを窒素ガス雰囲気中で行った場合にはN成分の含有量は高くなる(N:0.04質量%以上0.1質量%以下)。
Co成分は、本合金の主要成分の一つであり、最大含有率の成分である。前述したように、Co基合金材は、Ni基合金材と同等以上の耐食性や耐摩耗性を有する利点がある。
図2は本発明に係るCo基合金粉末およびCo基合金焼結体の製造方法の工程例を示すフロー図である。図2に示すように、まず、上述した本発明のCo基合金粉末の組成となるように、Co基合金粉末の原料を混合・溶解して溶湯10を形成する原料混合溶解工程(ステップ1:S1)を行う。溶解方法に特段の限定はなく、高耐熱合金に対する従前の方法(例えば、誘導溶解法、電子ビーム溶解法、プラズマアーク溶解法)を好適に利用できる。
図1は本発明のCo基合金粉末の粉末表面を模式的に示す図である。図1に示すように、本発明のCo基合金粉末20は、平均粉末粒径が5μm以上150μm以下の粉末21で構成される多結晶体であり、粉末21の表面及び内部には、偏析セル22が形成されている。偏析セル22は、後述するCo基合金粉末を製造する工程(粉末化工程)における冷却速度によって形が変わる。冷却速度が比較的速いと球状の偏析セルとなり、冷却速度が比較的遅いとデンドライト状(樹枝状)の偏析セルとなる。図1では、偏析セルがデンドライト状(樹枝状)である例を示している。Co基合金粉末20を焼結後、この偏析セルに沿って炭化物が析出されると考えられる。
本発明のCo基合金粉末の粒径は、5μm以上85μm以下であることが好ましい。より好ましくは10μm以上85μm以下であり、さらに好ましくは5μm以上25μm以下である。
図2に示すように、急冷凝固によって生成したCo基合金粉末20を焼結する焼結工程(ステップ3:S3)を行うことで、本発明のCo基合金焼結体を得ることができる。焼結方法に特に限定は無く、例えば熱間静水圧プレス(Hot Isostatic Pressing)を用いることができる。
表1のIA-2およびCA-5の粒度Sの合金粉末を用いてHIPにより成形体(直径8mm×高さ10mm)を形成した。HIPの焼結条件は、1150℃、150MPa、1時間とした。その後、980℃で4時間の熱処理を行い、IA-2粉末を用いた焼結体よびCA-5粉末を用いた焼結体を作製した。
上述したIA-2およびCA-5の粒度Lの合金粉末を用いて精密鋳造法により鋳造体(直径8mm×高さ10mm)を形成し、上記と同様の溶体化熱処理工程と時効熱処理工程とを行って、IA-2粉末を用いた鋳造合金製造物(鋳造体)およびCA-5粉末を用いた鋳造合金製造物(鋳造体)を作製した。
上記で作製した焼結体および鋳造体から、微細組織観察用および機械的特性試験用の試験片をそれぞれ採取し、微細組織観察および機械的特性試験を行った。
図3は、本発明のCo基合金製造物の一例であり、タービン高温部材としてのタービン静翼を示す斜視模式図である。図3に示したように、タービン静翼100は、概略的に、内輪側エンドウォール101と翼部102と外輪側エンドウォール103とから構成される。翼部の内部には、しばしば冷却構造が形成される。なお、例えば、出力30MW級の発電用ガスタービンの場合、タービン静翼の翼部の長さ(両エンドウォールの間の距離)は170mm程度である。
Claims (20)
- 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.003質量%以上0.04質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金粉末であり、
前記コバルト基合金粉末を構成する結晶粒が偏析セルを有し、前記偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とするコバルト基合金粉末。 - 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.04質量%より大きく0.1質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金粉末であり、
前記コバルト基合金粉末を構成する結晶粒が偏析セルを有し、前記偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とするコバルト基合金粉末。 - 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.04質量%より大きく0.1質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金粉末であり、
前記コバルト基合金粉末の粒径が5μm以上85μm以下であることを特徴とするコバルト基合金粉末。 - 前記コバルト基合金粉末の粒径が5μm以上85μm以下であることを特徴とする請求項1または2に記載のコバルト基合金粉末。
- 前記コバルト基合金粉末の粒径が5~25μmであることを特徴とする請求項1から3のいずれか1項に記載のコバルト基合金粉末。
- 前記コバルト基合金粉末の粒径が10~85μmであることを特徴とする請求項1から3のいずれか1項に記載のコバルト基合金粉末。
- 前記チタンを含む場合該チタンは0.01質量%以上1質量%以下であり、
前記ジルコニウムを含む場合該ジルコニウムは0.05質量%以上1.5質量%以下であり、
前記ニオブを含む場合該ニオブは0.02質量%以上1質量%以下であり、
前記タンタルを含む場合該タンタルは0.05質量%以上1.5質量%以下であり、
前記ハフニウムを含む場合該ハフニウムは0.01質量%以上0.5質量%以下であり、
前記バナジウムを含む場合該バナジウムは0.01質量%以上0.5質量%以下であることを特徴とする請求項1から3のいずれか1項に記載のコバルト基合金粉末。 - 不純物として、0.5質量%以下のアルミニウムと、0.04質量%以下の酸素とを含むことを特徴とする請求項1から3のいずれか1項に記載のコバルト基合金粉末。
- 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.003質量%以上0.04質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金焼結体であり、
前記コバルト基合金焼結体を構成する結晶粒が偏析セルを有し、前記偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とするコバルト基合金焼結体。 - 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.04質量%より大きく0.1質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金焼結体であり、
前記コバルト基合金焼結体を構成する結晶粒が偏析セルを有し、前記偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とするコバルト基合金焼結体。 - 0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムのうちの少なくとも1つを合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.04質量%より大きく0.1質量%以下の窒素とを含み、残部がコバルトと不純物とからなるコバルト基合金焼結体であり、
前記コバルト基合金焼結体の粒径が5μm以上85μm以下であることを特徴とするコバルト基合金焼結体。 - 前記コバルト基合金焼結体の粒径が5μm以上85μm以下であることを特徴とする請求項9または10に記載のコバルト基合金焼結体。
- 前記コバルト基合金焼結体の粒径が5μm以上25μm以下であることを特徴とする請求項9から11のいずれか1項に記載のコバルト基合金焼結体。
- 前記コバルト基合金焼結体の粒径が10μm以上85μm以下であることを特徴とする請求項9から11のいずれか1項に記載のコバルト基合金焼結体。
- 前記チタンを含む場合該チタンは0.01質量%以上1質量%以下であり、
前記ジルコニウムを含む場合該ジルコニウムは0.05質量%以上1.5質量%以下であり、
前記ニオブを含む場合該ニオブは0.02質量%以上1質量%以下であり、
前記タンタルを含む場合該タンタルは0.05質量%以上1.5質量%以下であり、
前記ハフニウムを含む場合該ハフニウムは0.01質量%以上0.5質量%以下であり、
前記バナジウムを含む場合該バナジウムは0.01質量%以上0.5質量%以下であることを特徴とする請求項9から11のいずれか1項に記載のコバルト基合金焼結体。 - 不純物として、0.5質量%以下のアルミニウムと、0.04質量%以下の酸素とを含むことを特徴とする請求項9から11のいずれか1項に記載のコバルト基合金焼結体。
- 前記偏析セルに炭化物が析出していることを特徴とする請求項9から11のいずれか1項に記載のコバルト基合金焼結体。
- 所定の化学組成を有するコバルト基合金粉末の原料を混合・溶解して溶湯を作製する原料混合溶解工程と、
前記溶湯から急冷凝固合金粉末を形成する溶湯-粉末化工程と、
前記急冷凝固合金粉末を焼結する焼結工程とを有し、
前記コバルト基合金粉末は、0.08質量%以上0.25質量%以下の炭素と、
0.1質量%以下のホウ素と、
10質量%以上30質量%以下のクロムと、
5質量%以下の鉄と、
30質量%以下のニッケルとを含み、
前記鉄と前記ニッケルを合計が30質量%以下となるように含み、
タングステンおよびモリブデンのうちの少なくとも1つを合計が5質量%以上12質量%以下となるように含み、
チタン、ジルコニウム、ニオブ、タンタル、ハフニウムおよびバナジウムの少なくとも1つの合計が0.5質量%以上2質量%以下となるように含み、
0.5質量%以下のケイ素と、
0.5質量%以下のマンガンと、
0.003質量%以上0.04質量%以下の窒素とを含み、残部がコバルトと不純物とからなり、前記コバルト基合金粉末を構成する結晶粒が偏析セルを有し、前記偏析セルの平均サイズが0.15μm以上4μm以下であることを特徴とするコバルト基合金焼結体の製造方法。 - 前記溶湯-粉末化工程は、ガスアトマイズまたはプラズマアトマイズによって前記急冷凝固合金粉末を形成することを特徴とする請求項18に記載のコバルト基合金焼結体の製造方法。
- コバルト基合金焼結体の原料は、前記コバルト基合金粉末を75質量%以上含むことを特徴とする請求項18または19に記載のコバルト基合金焼結体の製造方法。
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- 2019-12-26 KR KR1020217001718A patent/KR102435878B1/ko active IP Right Grant
- 2019-12-26 JP JP2020509116A patent/JP6938765B2/ja active Active
- 2019-12-26 AU AU2019432628A patent/AU2019432628B2/en active Active
- 2019-12-26 EP EP19848920.5A patent/EP3725901A4/en active Pending
- 2019-12-26 CA CA3105471A patent/CA3105471C/en active Active
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US11306372B2 (en) | 2022-04-19 |
RU2771192C1 (ru) | 2022-04-28 |
EP3725901A4 (en) | 2021-12-15 |
US20210140016A1 (en) | 2021-05-13 |
CA3105471A1 (en) | 2020-09-10 |
WO2020179082A1 (ja) | 2020-09-10 |
CN112004953A (zh) | 2020-11-27 |
KR20210022682A (ko) | 2021-03-03 |
AU2019432628B2 (en) | 2022-11-10 |
JP6938765B2 (ja) | 2021-09-22 |
AU2019432628A1 (en) | 2021-01-28 |
KR102435878B1 (ko) | 2022-08-24 |
EP3725901A1 (en) | 2020-10-21 |
CA3105471C (en) | 2022-12-13 |
JPWO2020179207A1 (ja) | 2021-03-11 |
SG11202100143WA (en) | 2021-09-29 |
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