WO2020121367A1 - Corps moulé stratifié en alliage à base de cobalt, produit en alliage à base de cobalt et leur procédé de fabrication - Google Patents

Corps moulé stratifié en alliage à base de cobalt, produit en alliage à base de cobalt et leur procédé de fabrication Download PDF

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WO2020121367A1
WO2020121367A1 PCT/JP2018/045245 JP2018045245W WO2020121367A1 WO 2020121367 A1 WO2020121367 A1 WO 2020121367A1 JP 2018045245 W JP2018045245 W JP 2018045245W WO 2020121367 A1 WO2020121367 A1 WO 2020121367A1
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mass
based alloy
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cobalt
alloy powder
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Japanese (ja)
Inventor
今野　晋也
玉艇 王
滋信 江口
上村　好古
宜彦 本山
孝直 小牧
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Mitsubishi Power Ltd
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Mitsubishi Hitachi Power Systems Ltd
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Priority to CA3061851A priority Critical patent/CA3061851C/fr
Priority to AU2018422117A priority patent/AU2018422117B2/en
Priority to PCT/JP2018/045245 priority patent/WO2020121367A1/fr
Publication of WO2020121367A1 publication Critical patent/WO2020121367A1/fr
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present invention relates to a cobalt-based alloy material having excellent mechanical properties, and particularly to a cobalt-based alloy laminate-molded product, a cobalt-based alloy product based on the laminate-molded product, and a manufacturing method thereof.
  • Cobalt (Co)-based alloy materials are typical heat-resistant alloy materials along 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. Co-based alloy materials have higher material costs than Ni-based alloy materials, but are superior in corrosion resistance and wear resistance and are easily solid-solution strengthened, and thus have been used as turbine vanes and combustor members.
  • Ni-based alloy materials are strengthened by precipitation of the ⁇ 'phase (for example, Ni 3 (Al,Ti) phase).
  • ⁇ 'phase for example, Ni 3 (Al,Ti) phase.
  • Co-based alloy materials it is difficult to precipitate an intermetallic compound phase that greatly contributes to the improvement of mechanical properties such as the ⁇ ′ phase of Ni-based alloy materials, so precipitation strengthening by a carbide phase has been studied.
  • Patent Document 1 JP-A-61-243143
  • bulk and granular carbides having a grain size of 0.5 to 10 ⁇ m are deposited on a matrix of a cobalt-based alloy having a grain size of 10 ⁇ m or less.
  • a Co-based superplastic alloy characterized by the following is disclosed. Further, 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: It is disclosed that 0 to 1.0%, Zr: 0 to 1.0%, Ta: 0 to 1.0%, Ti: 0 to 3%, Al: 0 to 3%, and the balance Co.
  • Co-based superplasticity that exhibits superplasticity even in a low temperature region (for example, 950° C.) and has an elongation of 70% or more, and that a complex-shaped object can be produced by plastic working such as forging It is said that it can provide alloys.
  • Patent Document 2 JP-A-7-17967
  • Cr 21-29%
  • Mo 15-24%
  • B 0.5-2%
  • Si 0.1% or more and less than 0.5%
  • C by weight% A Co-based alloy having excellent corrosion resistance, wear resistance and high temperature strength, which comprises more than 1% and 2% or less, Fe: 2% or less, Ni: 2% or less and the balance substantially Co, is disclosed.
  • 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 corrosion resistance. It is said to have wear resistance and high strength.
  • 3D printing such as additive manufacturing (AM method) has attracted attention as a technology for manufacturing a final product having a complicated shape in a near net shape.
  • AM method additive manufacturing
  • Patent Document 3 Japanese Patent Publication No. 2016-535169
  • a layer forming method including the following steps: a) A raw material of a powdery or suspension granular composite material having a porosity of less than 20% is supplied. B) depositing a first portion of the composite material on a target surface, c) supplying energy to the composite material of the first portion to sinter, fuse, or fuse the first portion of the composite material.
  • the selective laser melting method (SLM method) or the direct metal laser melting method (DMLM method) generally uses one material (pure titanium or Ti-6Al-4V). Such a single alloy) is beneficial.
  • SLS selective laser sintering
  • DMLS direct metal laser sintering
  • 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 when compared with the recent precipitation-strengthened Ni-based alloy materials. Unfortunately, it does not have sufficient mechanical properties. For this reason, at present, most of the research on additive-molded products (AM products) for high-temperature turbine applications is aimed at precipitation-strengthened Ni-based alloy materials.
  • AM products additive-molded products
  • AM bodies of precipitation-strengthened Ni-based alloys are liable to cause defects such as the inhibition of the generation of the ⁇ 'phase, which is a key to the mechanical properties, and the occurrence of internal defects in the product, and are expected as a result.
  • mechanical properties cannot be sufficiently obtained. This is because the current precipitation-strengthened Ni-based alloy materials used as high-temperature turbine components are optimized on the premise of the melting/casting process in high vacuum. It is considered that the Al component and the Ti component constituting the ⁇ ′ phase are likely to be oxidized or nitrided at the stage of the AM method.
  • the Co-based alloy materials described in Patent Documents 1 and 2 are not premised on the precipitation of an intermetallic compound phase such as the ⁇ ′ phase of the Ni-based alloy material. It does not contain much, and the melting/casting process in the atmosphere can be used. Therefore, it is considered to be advantageous for the production of alloy powder for the AM method and the production of AM bodies. Further, 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 conventional Co-based alloy material has a weak point that it has lower mechanical properties than the ⁇ 'phase precipitation strengthened Ni-based alloy material.
  • achieve mechanical properties equivalent to or higher than those of ⁇ 'phase precipitation strengthened Ni-based alloy materials for example, creep resistance temperature of 875°C for 100,000 hours at 58 MPa, tensile strength at room temperature of 500 MPa or more. If so, the Co-based alloy AM body can be a very attractive turbine high temperature member.
  • the present invention has been made in view of the above problems, and its purpose is as a Co-based alloy material having a mechanical property equal to or higher than that of a precipitation-strengthened Ni-based alloy material, a Co-based alloy layered article, It is an object of the present invention to provide a Co-based alloy product based on the layered product and a method for producing the same.
  • Co-based alloy is 0.08 mass% or more and 0.25 mass% or less of carbon (C), 0.1 mass% or less of boron (B), 10% by mass or more and 30% by mass or less of chromium (Cr), Iron and nickel (Ni) with iron (Fe) of 5 mass% or less and total of 30 mass% or less, Tungsten (W) and/or molybdenum (Mo) in a total amount of 5% by mass or more and 12% by mass or less, Titanium (Ti), zirconium (Zr), niobium (Nb) and tantalum (Ta) with a total amount of 0.5% by mass or more and 2% by mass or less, 0.5% by mass or less of silicon (Si), 0.5% by mass or less of manganese (Mn), Contains 0.003 mass% or more and 0.04 mass% or less nitrogen (N), The balance has a chemical composition consisting of Co and
  • the following segregation cells are formed, and/or the particles of the MC type carbide phase are precipitated at an average interparticle distance of 0.15 ⁇ m or more and 1.5 ⁇ m or less,
  • the present invention provides a Co-based alloy layered product characterized by the above.
  • the chemical composition of the Co-based alloy is such that the Ti is 0.01% by mass or more and 1% by mass or less, the Zr is 0.05% by mass or more and 1.5% by mass or less, and the Nb is 0.02% by mass or more and 1% by mass. % Or less, and the Ta is 0.05% by mass or more and 1.5% by mass or less.
  • the chemical composition of the Co-based alloy contains 0.5% by mass or less of aluminum (Al) and 0.04% by mass or less of oxygen (O) as the impurities.
  • the Co-based alloy is C of 0.08 mass% or more and 0.25 mass% or less, B of 0.1 mass% or less, 10 mass% or more and 30 mass% or less of Cr, Fe and Ni with Fe of 5 mass% or less and total of 30 mass% or less, W and/or Mo whose total is 5% by mass or more and 12% by mass or less, Ti, Zr, Nb, and Ta whose total is 0.5% by mass or more and 2% by mass or less, 0.5 mass% or less of Si, Mn of 0.5 mass% or less, Including 0.003 mass% or more and 0.04 mass% or less N,
  • the balance has a chemical composition consisting of Co and impurities
  • the product is a polycrystal having an average crystal grain size of 20 ⁇ m or more and 145 ⁇ m or less, In the crystal grains of the polycrystalline body, particles of the MC type carbide phase containing Ti, Zr, Nb and/or Ta
  • the above-mentioned product has a room temperature 0.2% proof stress of 500 MPa or more and a creep durability temperature of 875° C. or more that does not break at a stress of 58 MPa for 100,000 hours.
  • the chemical composition of the Co-based alloy is such that the Ti is 0.01% by mass or more and 1% by mass or less, the Zr is 0.05% by mass or more and 1.5% by mass or less, and the Nb is 0.02% by mass or more and 1% by mass. % Or less, and the Ta is 0.05% by mass or more and 1.5% by mass or less.
  • the chemical composition of the Co-based alloy contains 0.5% by mass or less of Al and 0.04% by mass or less of O as the impurities.
  • the product is a turbine high temperature member.
  • the turbine high temperature member is a turbine vane or a combustor nozzle.
  • Yet another aspect of the present invention is a method for producing the above Co-based alloy laminated body, An alloy powder preparing step of preparing a Co-based alloy powder having the chemical composition, An alloy powder bed preparation step of preparing an alloy powder bed having a predetermined thickness by spreading the Co-based alloy powder, and irradiating a predetermined region of the alloy powder bed with a laser beam to obtain the Co-based alloy powder in the region.
  • the present invention provides a method for producing a Co-based alloy laminate-molded body characterized by the above.
  • the present invention can be modified and changed as described below in the method (III) for manufacturing a Co-based alloy laminated body.
  • the alloy powder preparing step includes an alloy powder classifying step for classifying the Co-based alloy powder into a particle size range of 5 ⁇ m or more and 100 ⁇ m or less.
  • Yet another aspect of the present invention is a method for producing the above Co-based alloy product, An alloy powder preparing step of preparing a Co-based alloy powder having the chemical composition, An alloy powder bed preparation step of preparing an alloy powder bed having a predetermined thickness by spreading the Co-based alloy powder, and irradiating a predetermined region of the alloy powder bed with a laser beam to obtain the Co-based alloy powder in the region.
  • the laminate-molded body has a solution heat treatment step of performing solution treatment for a holding time of 0.5 hours or more and 10 hours or less in a temperature range of 1100° C. or more and 1200° C.
  • the SLM step the relationship between the predetermined thickness h (unit: ⁇ m) of the alloy powder bed, the output P (unit: W) of the laser light, and the scanning speed S (unit: mm/s) of the laser light. So that “15 ⁇ h ⁇ 150” and “67(P/S) ⁇ 3.5 ⁇ h ⁇ 2222(P/S)+13” are satisfied, the predetermined thickness h, the output P, and the scanning speed S are Control,
  • a method for producing a Co-based alloy product comprising:
  • the present invention can make the following improvements and changes in the above-mentioned production method (IV) of a Co-based alloy product.
  • the alloy powder preparing step includes an alloy powder classifying step for classifying the Co-based alloy powder into a particle size range of 5 ⁇ m or more and 100 ⁇ m or less.
  • an aging heat treatment step of subjecting the laminate-molded body to an aging treatment in a temperature range of 750° C. to 1000° C. for a holding time of 0.5 hours to 10 hours.
  • a Co-based alloy material having mechanical properties equal to or higher than that of a precipitation-strengthened Ni-based alloy material a Co-based alloy laminate-molded product, a Co-based alloy product based on the laminate-molded product, and those Can be provided.
  • FIG. 1 is a scanning electron microscope (SEM) observation image showing an example of a microstructure of a Co-based alloy AM body according to the present invention.
  • 1 is an example of a Co-based alloy product according to the present invention, and is a schematic perspective view showing a turbine vane as a turbine high temperature member.
  • 1 is a schematic cross-sectional view showing an example of a gas turbine equipped with a Co-based alloy product according to the present invention.
  • 3 is an SEM observation image showing an example of a microstructure of a Co-based alloy AM body formed by a laser metal deposition method (LMD method).
  • LMD method laser metal deposition method
  • FIG. 3 is an SEM observation image showing an example of a microstructure of a Co-based alloy cast body formed by a precision casting method. 3 is a graph showing an example of the relationship between the average size of segregation cells in a Co-based alloy AM body and 0.2% proof stress in a Co-based alloy product.
  • FIG. 4 is an SLM condition example for obtaining a Co-based alloy AM body according to the present invention, and is a graph showing the relationship between the thickness of the alloy powder bed and the local heat input.
  • the components of Ti, Zr, Nb, and Ta, which are indispensable for forming the carbide phase, are notable at the final solidification part (eg, dendrite boundary or grain boundary) during melt solidification of the Co-based alloy.
  • the carbide phase particles are precipitated along the dendrite boundaries and the crystal grain boundaries of the matrix phase.
  • the average spacing of dendrite boundaries and the average grain size are usually in the order of 10 1 to 10 2 ⁇ m in ordinary cast Co-based alloy materials, so the average spacing of the carbide phase particles is also in the order of 10 1 to 10 2 ⁇ m.
  • the average spacing of the carbide phase particles in the solidified portion is about 5 ⁇ m.
  • precipitation strengthening in an alloy is inversely proportional to the average distance between precipitates, and precipitation strengthening is said to be effective when the average distance between precipitates is about 2 ⁇ m or less.
  • the average distance between the precipitates does not reach the level, and the effect of sufficient precipitation strengthening cannot be obtained.
  • Cr carbide phase is another carbide phase that can be precipitated in Co-based alloys. Since the Cr component has a high solid solubility in the Co-based alloy matrix and is difficult to segregate, the Cr carbide phase can be dispersed and precipitated in the matrix crystal grains. However, it is known that the Cr carbide phase has low lattice matching with the Co-based alloy matrix crystal and is not so effective as a precipitation strengthening phase.
  • the present inventors in the Co-based alloy material, if it is possible to disperse and precipitate the carbide phase particles that contribute to precipitation strengthening in the matrix crystal grains, it is possible to dramatically improve the mechanical properties of the Co-based alloy material. I thought I could do it. In addition, 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 diligently studied the alloy composition and manufacturing method for obtaining such a Co-based alloy material. As a result, by optimizing the alloy composition and controlling the heat input for local melting and rapid solidification within a predetermined range in the manufacturing using the AM method (particularly, selective laser melting method), It has been found that carbide phase particles that contribute to alloy strengthening can be dispersed and precipitated in the matrix crystal grains of the alloy material. The present invention has been completed based on this finding.
  • FIG. 1 is a flow chart showing a process example of a method for producing a Co-based alloy product according to the present invention.
  • the method for producing a Co-based alloy product according to the present invention roughly uses an alloy powder preparing step (S1) for preparing Co-based alloy powder and the prepared Co-based alloy powder.
  • Selective laser melting step (S2) to form an AM body with a desired shape
  • solution heat treatment step (S3) to subject the formed AM body to solution treatment
  • S4 an aging heat treatment step of applying an aging treatment.
  • the AM body obtained by the selective laser melting step S2 is the Co-based alloy laminate-molded body according to the present invention.
  • This step S1 is a step of preparing a Co-based alloy powder having a predetermined chemical composition.
  • the chemical composition is 0.08 mass% or more and 0.25 mass% or less C, 0.1 mass% or less B, 10 mass% or more and 30 mass% or less Cr, and Fe is 5 mass% or less and the total is 30 mass% or less.
  • Fe and Ni, W and/or Mo in total 5 mass% to 12 mass%, Ti, Zr, Nb and Ta in total 0.5 mass% to 2 mass% and 0.5 mass% or less Si And 0.5% by mass or less of Mn and 0.003% by mass or more and 0.04% by mass or less of N, with the balance being Co and impurities.
  • the C component constitutes an MC type carbide phase (which may be referred to as a Ti, Zr, Nb and/or Ta carbide phase or a strengthened carbide phase) which is a precipitation strengthening phase. It is an ingredient.
  • 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 further preferably 0.12 mass% or more and 0.18 mass% or less. If the C content is less than 0.08 mass %, the amount of precipitation of the strengthened carbide phase will be insufficient, and the effect of improving the mechanical properties will not be sufficiently obtained. On the other hand, if the C content exceeds 0.25% by mass, excessive hardening causes the ductility and toughness of the alloy material to decrease.
  • Component B is a component that contributes to the improvement of the bondability of crystal grain boundaries (so-called grain boundary strengthening). Although the B component is not an essential component, when it is contained, it is preferably 0.1% by mass or less, more preferably 0.005% by mass or more and 0.05% by mass or less. If the B content exceeds 0.1 mass %, cracks (for example, solidification cracks) tend to occur during formation of the AM body.
  • the Cr component is a component that contributes to improvement in 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 Cr content 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, if the Cr content exceeds 30 mass %, brittle ⁇ phase or Cr carbide phase is generated and mechanical properties (toughness, ductility, strength) are deteriorated.
  • 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 replacing a part of the Co component.
  • the Ni component is not an essential component, but when contained, it is preferably 30% by mass or less, more preferably 20% by mass or less, further preferably 5% by mass or more and 15% by mass or less. If the Ni content exceeds 30 mass %, the wear resistance and 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 fault 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, and therefore, it is a component that can be contained by replacing a part of the Ni component. That is, the total content of Fe and Ni is preferably 30 mass% or less, more preferably 20 mass% or less, and further preferably 5 mass% or more and 15 mass% or less.
  • the Fe component is not an essential component, but when it is contained, it is preferably 5% by mass or less, 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 5 mass% or more and 12 mass% or less in total W component and Mo component are components that contribute to solid solution strengthening of the matrix phase.
  • 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.
  • the total content of the W component and the Mo component is less than 5% by mass, the solid solution strengthening of the matrix becomes insufficient.
  • the total content of the W component and the Mo component exceeds 12 mass %, a brittle ⁇ phase is likely to be formed and mechanical properties (toughness, ductility) are deteriorated.
  • Re component 2% by mass or less Re component is a component that contributes to solid solution strengthening of the matrix 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 and 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 the Mo component. If the Re content exceeds 2% by mass, not only the action and effect of the Re component will be saturated, but also the material cost will increase.
  • Ti, Zr, Nb and Ta 0.5% by mass or more and 2% by mass or less in total Ti component, Zr component, Nb component and Ta component are important components constituting the strengthened carbide phase (MC type carbide phase).
  • the total content of Ti, Zr, Nb, and Ta 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. If the total content is less than 0.5% by mass, the amount of precipitation of the strengthened carbide phase will be insufficient, and the effect of improving the mechanical properties will not be sufficiently obtained. On the other hand, when the total content exceeds 2% by mass, the reinforced carbide phase particles become coarse or accelerate the generation of brittle phase (for example, ⁇ phase) or generate oxide phase particles that do not contribute to precipitation strengthening. Mechanical properties deteriorate.
  • the Ti content is preferably 0.01% by mass or more and 1% by mass or less, more preferably 0.05% by mass or more and 0.8% by mass or less.
  • the Zr 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 Nb content is preferably 0.02% by mass or more and 1% by mass or less, more preferably 0.05% by mass or more and 0.8% by mass or less.
  • the Ta 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 Si component plays a role of deoxidizing 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 oxide (for example, SiO 2 ) are formed, which causes a decrease in mechanical properties.
  • the Mn component is a component that plays a role of deoxygenation/desulfurization and contributes to improvement of mechanical properties and corrosion resistance.
  • the Mn 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 Mn content exceeds 0.5 mass %, coarse particles of sulfide (for example, MnS) are formed, which causes a decrease in mechanical properties and corrosion resistance.
  • the N component is a component that contributes to stable formation of a strengthened carbide phase.
  • the content of the N component is preferably 0.003 mass% or more and 0.04 mass% or less, more preferably 0.005 mass% or more and 0.03 mass% or less, and further preferably 0.007 mass% or more and 0.025 mass% or less. If the N content is less than 0.003% by mass, the effect of the N component cannot be sufficiently obtained. On the other hand, when the N content exceeds 0.04 mass %, coarse particles of nitride (eg, Cr nitride) are formed, which becomes a factor of lowering mechanical properties.
  • nitride eg, Cr nitride
  • Co component + impurities Co component is one of the main components of this alloy, and is the component with the maximum content.
  • 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 0.3 mass% or less is acceptable because it does not have a significant adverse effect on the mechanical properties of the Co-based alloy product. If the Al content exceeds 0.3% by mass, coarse particles of oxides or nitrides (for example, Al 2 O 3 or AlN) are formed, which causes deterioration of 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 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 O content exceeds 0.04% by mass, coarse particles of various oxides (eg, Ti oxide, Zr oxide, Al oxide, Fe oxide, Si oxide) will be formed and cause deterioration of mechanical properties. become.
  • various oxides eg, Ti oxide, Zr oxide, Al oxide, Fe oxide, Si oxide
  • step S1 there is no particular limitation on the method/method for preparing the Co-based alloy powder, and the conventional method/method can be used.
  • the atomizing process (S1b) may be performed.
  • the atomizing method is not particularly limited, and the conventional method/method can be used.
  • a gas atomizing method or a centrifugal atomizing method which can obtain spherical particles having a high purity, a homogeneous composition, can be preferably used.
  • the particle size of the alloy powder is preferably 5 ⁇ m or more and 100 ⁇ m or less, more preferably 10 ⁇ m or more and 70 ⁇ m or less, and more preferably 10 ⁇ m or more and 50 ⁇ m or less, from the viewpoint of handleability and filling property of the alloy powder bed in the selective laser melting step S2 of the next step. More preferable. If the particle size of the alloy powder is less than 5 ⁇ m, the fluidity of the alloy powder is reduced in the next step S2 (the formability of the alloy powder bed is reduced), which is a factor that reduces the shape accuracy of the AM body.
  • the alloy powder classifying step (S1c) for classifying the particle size of the alloy powder in the range of 5 ⁇ m or more and 100 ⁇ m or less.
  • the element step S1c has been performed.
  • This step S2 is a step of forming an AM body having a desired shape by the selective laser melting (SLM) method using the prepared Co-based alloy powder.
  • SLM selective laser melting
  • S2b laser melting and solidifying element step
  • step S2 in order to obtain the desired fine structure (fine structure in which the strengthening carbide phase particles are dispersed and precipitated in the matrix phase crystal grains) in the final Co-based alloy product, it becomes the precursor of the product AM Controls the microstructure of the body. Then, in order to control the fine structure of the AM body, local melting and rapid solidification of the alloy powder bed are controlled.
  • the alloy powder bed thickness h (unit: ⁇ m) of the alloy powder bed, the laser beam output P (unit: W), and the laser beam scanning speed S (unit: mm/s), “15 ⁇ h ⁇ 150” and “67(P/S)-3.5 ⁇ h ⁇ 2222(P/S)+13”, the alloy powder bed thickness h, laser light output P, laser light scanning speed S and Is preferably controlled. If the control conditions are not satisfied, an AM body having a desired fine structure cannot be obtained. By this step S2, the Co-based alloy AM body according to the present invention is obtained.
  • the output P of the laser light and the scanning speed S of the laser light basically depend on the configuration of the laser device, but can be selected within the range of, for example, "10 ⁇ P ⁇ 1000" and "10 ⁇ S ⁇ 7000". Good.
  • FIG. 2 is a scanning electron microscope (SEM) observation image showing an example of the microstructure of the Co-based alloy AM body according to the present invention. As shown in FIG. 2, the Co-based alloy AM body of the present invention has an extremely specific microstructure that has never been seen before.
  • the AM body is a polycrystalline body having an average crystal grain size of 10 ⁇ m or more and 100 ⁇ m or less, and a segregation cell having an average size of 0.15 ⁇ m or more and 1.5 ⁇ m or less is formed in the crystal grains of the polycrystalline body. Further, particles of a strengthened carbide phase are precipitated at an average interval of 0.15 ⁇ m or more and 1.5 ⁇ m or less.
  • the segregation cell size is defined as the average of the major axis and the minor axis.
  • TEM-EDX transmission electron microscope-energy dispersive X-ray spectroscopy
  • This step S3 is a step of subjecting the formed Co-based alloy AM body to solution treatment.
  • solution treatment conditions heat treatment is preferably performed in a temperature range of 1100° C. or more and 1200° C. or less and a holding time of 0.5 hour or more and 10 hours or less.
  • the cooling method after the heat treatment is not particularly limited, and any of water cooling, oil cooling, air cooling, and furnace cooling may be used.
  • the average crystal grain size of the mother phase crystal grains is controlled to a range of 20 ⁇ m or more and 145 ⁇ m or less by recrystallization.
  • the average crystal grain size is less than 20 ⁇ m or more than 145 ⁇ m, sufficient creep properties cannot be obtained in the final Co-based alloy product.
  • the components segregated in the boundary region of the previous segregation cell start to aggregate to form a strengthened carbide phase, and as a result, the segregation cell is It disappeared (more precisely, the segregation cell could not be confirmed by SEM observation).
  • the agglomeration point at which the strengthened carbide phase begins to form is considered to be the triple point/four-point position of the original segregation cell boundary, and it is in a state of being finely distributed throughout the matrix grains (inside the grains and on the grain boundaries). Become.
  • the Co-based alloy product may be completed in this step S3.
  • This step S4 is a step of subjecting the Co-based alloy AM body that has been subjected to the solution treatment to an aging treatment.
  • the aging treatment condition heat treatment with a holding time of 0.5 hours to 10 hours in a temperature range of 750° C. to 1000° C. is preferable.
  • the cooling method after the heat treatment is not particularly limited, and any of water cooling, oil cooling, air cooling, and furnace cooling may be used.
  • the strengthened carbide phase that started to form in the solution heat treatment step S3 into the form of particles while suppressing excessive coarsening of the matrix phase crystal grains.
  • the average crystal grain size of the mother phase crystal grains is 20 ⁇ m or more and 145 ⁇ m or less
  • the reinforcing carbide phase particles are finely dispersed and precipitated in each crystal grain
  • the average interparticle distance of the reinforcing carbide phase particles is 0.15 ⁇ m. It is possible to obtain a Co-based alloy product having a size of 1.5 ⁇ m or less.
  • the strengthened carbide phase particles are dispersed and precipitated also on the grain boundaries of the parent phase crystal grains.
  • a step of forming a corrosion-resistant coating layer or a surface finishing step on the Co-based alloy product obtained by the solution heat treatment step S3 or the aging heat treatment step S4. May be further performed.
  • FIG. 3 is an example of a Co-based alloy product according to the present invention, and is a schematic perspective view showing a turbine vane as a turbine high temperature member.
  • the turbine vane 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. As described above, since the turbine vane 100 has a very complicated shape and structure, the technical significance of the AM body formed by the near net shape and the alloy product based on the AM body is great.
  • the length of the blade portion of the turbine vane (distance between both end walls) is about 170 mm.
  • FIG. 4 is a schematic 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 composed of a compressor section 210 that compresses intake air and a turbine section 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 the turbine nozzle 221 in the turbine section 220 or the turbine vane 100.
  • the turbine hot component of the present invention is not limited to gas turbine applications, but may be other turbine applications (eg, steam turbine applications).
  • alloy powder preparation step S1 Preparation of alloy powder IA-1 to IA-5 and CA-1 to CA-5) Co-based alloy powders having the chemical compositions shown in Table 1 were prepared (alloy powder preparation step S1). More specifically, first, after mixing the raw materials, a master alloy ingot producing step S1a of producing a master alloy ingot (mass: about 2 kg) by melting and casting by a vacuum high frequency induction melting method was performed. Next, the atomizing element step S1b of remelting the mother alloy ingot and forming alloy powder by a gas atomizing method in an argon gas atmosphere was performed.
  • an alloy powder classifying step S1c for controlling the particle size was performed on each of the obtained alloy powders.
  • an alloy powder whose particle size was classified into the range of 10 to 25 ⁇ m (particle size S) and an alloy powder classified into the range of 100 to 150 ⁇ m (particle size L) were prepared.
  • the alloy powders IA-1 to IA-5 are alloy powders having a chemical composition satisfying the regulations of the present invention.
  • the C content rate and the Cr content rate are out of the regulation of the present invention.
  • the C content rate, the Ni content rate, and the total content rate of “Ti+Zr+Nb+Ta” are out of the regulation of the present invention.
  • the alloy powder CA-3 the N content and the total content of “Ti+Zr+Nb+Ta” are out of the regulation of the present invention.
  • the alloy powder CA-4 the total content of “Ti+Zr+Nb+Ta” is out of the range of the present invention.
  • the W content and the total content of “Ti+Zr+Nb+Ta” are out of the regulation of the present invention.
  • Example 2 (Production of SLM alloy products using IA-2 powder and SLM alloy products using CA-5 powder) An AM body (diameter 8 mm ⁇ height 10 mm) was formed by the SLM method using the alloy powder of IA-2 and CA-5 having the grain size S prepared in Experiment 1 (selective laser melting step S2).
  • the control of the local heat input amount corresponds to the control of the cooling rate.
  • Each of the AM bodies produced above was heat-treated by holding it at 1150°C for 4 hours (solution heat treatment step S3).
  • the solution treated AM bodies were heat-treated at 900° C. for 4 hours (aging heat treatment step S4) to produce SLM alloy products using IA-2 powder and CA-5 powder.
  • An SLM alloy product using was prepared.
  • LMD alloy product using IA-2 powder and LMD alloy product using CA-5 powder An AM body was formed by the laser metal deposition method (LMD method) using the alloy powder of IA-2 and CA-5 having the grain size L prepared in Experiment 1, and the solution heat treatment step S3 and the aging heat treatment step S4 similar to the above By performing the above, an LMD alloy product using IA-2 powder and an LMD alloy product using CA-5 powder were produced.
  • the LMD conditions were a laser light output P of 800 W and a laser light scanning speed S of 15 mm/s.
  • the LMD method is a type of AM method, and is a method of additive manufacturing by performing alloy powder injection and laser irradiation at the same time.
  • the local heat input of the LMD method is generally larger than the local heat input of the SLM method. In other words, the cooling rate in the LMD method becomes slower than that in the SLM method.
  • a casting (diameter 8 mm x height 10 mm) was formed by precision casting using the alloy powder of IA-2 and CA-5 with grain size L prepared in Experiment 1, and the solution heat treatment step S3 similar to the above And an aging heat treatment step S4 were performed to produce a cast alloy product using the IA-2 powder and a cast alloy product using the CA-5 powder.
  • Microstructure observation and mechanical property test Specimens for microstructure observation and mechanical property test were taken from the AM body, cast body, and manufactured product produced above, respectively, and microstructure observation and mechanical property test were performed.
  • FIG. 5 is an SEM observation image showing an example of the microstructure of a Co-based alloy AM body formed by the LMD method
  • FIG. 6 is an SEM showing an example of the microstructure of a Co-based alloy cast body formed by the precision casting method. It is an observed image.
  • FIG. 2 shown above is an SEM observation image showing an example of the microstructure of the Co-based alloy AM body formed by the SLM method. The samples shown in FIGS. 2, 5 and 6 all use IA-2 as the alloy powder.
  • the AM body formed by the SLM method has a segregation cell of about 1 ⁇ m size formed within the crystal grains of the polycrystalline body.
  • the AM body formed by the LMD method is composed of a segregation cell in which each crystal grain of the polycrystalline body has a size of about 5 to 20 ⁇ m.
  • the cast body formed by the precision casting method see FIG. 6
  • microsegregation along the dendrite boundary was observed, and the interval of the microsegregation was about 100 to 300 ⁇ m.
  • the average interparticle distance is It was found that the average size and the average interval of microsegregation were almost the same (illustration of the microstructure is omitted).
  • solution treatment and aging treatment combine adjacent carbide phases to form large particles (as a result, It was found that the average interparticle distance of the carbide phase particles increases).
  • FIG. 7 is a graph showing an example of the relationship between the average size of segregation cells in a Co-based alloy AM body and 0.2% proof stress in a Co-based alloy product. Note that FIG. 7 also shows data of a cast body and a cast alloy product for comparison. In the cast body, the average size of the segregation cells was substituted by the average interval of microsegregation.
  • the Co-based alloy product produced using the CA-5 powder showed almost constant 0.2% proof stress without being affected by the average size of the segregation cell.
  • the Co-based alloy product produced using IA-2 powder had a large change in 0.2% proof stress depending on the average size of the segregation cell.
  • CA-5 powder has an excessively low total content of “Ti+Zr+Nb+Ta” (almost not included). Therefore, the product using the CA-5 powder had a fine structure in which the Cr carbide particles were precipitated without the precipitation of the strengthened carbide phase. This result confirms that Cr carbide particles are not very effective as precipitation strengthening particles. On the other hand, the product 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 greatly changed depending on the average size of the segregation cell (the average interparticle distance of the carbide phase particles as a result).
  • the 0.2% proof stress is required to be 500 MPa or more. Therefore, if a 0.2% proof stress of 500 MPa or more is judged as "pass” and less than 500 MPa is judged as "fail", the average size of the segregation cell (the resulting average interparticle distance of the carbide phase particles) is 0.15. It was confirmed that a mechanical property of “passing” was obtained in the range of up to 1.5 ⁇ 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.
  • Microstructure observation and mechanical property test From the SLM alloy products IP-1-1 to IP-5-1 and CP-1-1 to CP-5-1 produced above, sample specimens for microstructure observation and mechanical property test were collected. , Microstructure observation and mechanical property test were performed.
  • a creep test was performed under the conditions of a temperature of 900°C and a stress of 98 MPa, and the creep rupture time was measured. From the required characteristics of the turbine high temperature member targeted by the present invention, a creep rupture time of 1100 hours or more was determined as "pass", and a creep rupture time of less than 1100 hours was determined as "fail”.
  • a creep property that passes the test means that the temperature at which the creep rupture time is 100,000 hours at a stress of 58 MPa is 875°C or higher. It can be said that this creep characteristic is the same as that of the Ni-based alloy material.
  • CP-1-1 and CP-3-1 From the results of CP-1-1 and CP-3-1, it is confirmed that Cr carbide particles are not so effective as precipitation strengthening particles.
  • CP-4-1 and CP-5-1 are considered to be due to the fact that the strengthened carbide phase itself did not precipitate, because the total content of “Ti+Zr+Nb+Ta” was too small (because it was almost not included). Be done.
  • the average grain size of the matrix crystal grains is preferably 20 to 145 ⁇ m.
  • the solution treatment is preferably a heat treatment in which the temperature is maintained in the temperature range of 1100 to 1200° C. for 0.5 to 10 hours.
  • microstructure of each AM body prepared above was observed to measure the average size of the segregation cells.
  • SEM and image processing software were used as in Experiment 2.
  • FIG. 8 is an example of SLM conditions for obtaining the Co-based alloy AM body according to the present invention, and is a graph showing the relationship between the thickness of the alloy powder bed and the local heat input.
  • FIG. 8 as a result of observing the microstructure of the AM body, those having an average size of the segregation cell in the range of 0.15 to 1.5 ⁇ m were judged as “pass” and indicated by “ ⁇ ” in the figure, and other It was judged as "fail” and indicated by “x” in the figure.
  • the SLM conditions in the selective laser melting step S2 are as follows: the alloy powder bed thickness h (unit: ⁇ m), laser light output P (unit: W), and laser light scanning speed S (unit: It is confirmed that it is preferable to control so that the relationship with (mm/s) satisfies “15 ⁇ h ⁇ 150” and “67(P/S)-3.5 ⁇ h ⁇ 2222(P/S)+13”. .. That is, the hatched area is the area for acceptance determination.
  • Turbine stationary blade 101... Inner ring side end wall, 102... Blade section, 103... Outer ring side end wall, 200... Gas turbine, 210... Compressor section, 220... ..Turbine part, 221... Turbine nozzle

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Abstract

L'objectif de la présente invention est de fournir un corps moulé stratifié en alliage à base de Co qui est un matériau d'alliage à base de Co qui présente des caractéristiques mécaniques identiques ou meilleures par rapport à des matériaux d'alliage à base de Ni renforcés par précipitation, un produit d'alliage à base de Co basé sur ledit corps moulé stratifié, et leur procédé de fabrication. Ce produit d'alliage à base de Co est caractérisé en ce qu'il a une composition chimique qui contient de 0,08 à 0,25 % en masse de C, 0,1 % en masse ou moins de B, de 10 à 30 % en masse de Cr, Fe et Ni, Fe étant inférieur ou égal à 5 % en masse et le total inférieur ou égal à 30 % en masse, un total de 5 à 12 % en masse de W et/ou de Mo, un total de 0,5 à 2 % en masse de Ti, Zr, Nb et Ta, 0,5 % en masse ou moins de Si, 0,5 % en masse ou moins de Mn, et 0,003 à 0,04 % en masse de N, le reste étant du Co et des impuretés, et en ce que le produit susmentionné est un polycristal ayant une taille de grain cristallin moyenne de 20 à 145 µm, et à l'intérieur des grains cristallins du polycristal, des particules de phase de carbure de type MC, qui contiennent les Ti, Zr, Nb et/ou Ta susmentionnés, sont précipitées avec une distance moyenne entre particules de 0,15 à 1,5 µm.
PCT/JP2018/045245 2018-12-10 2018-12-10 Corps moulé stratifié en alliage à base de cobalt, produit en alliage à base de cobalt et leur procédé de fabrication Ceased WO2020121367A1 (fr)

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JP2023051722A (ja) * 2021-09-30 2023-04-11 三菱重工業株式会社 コバルト基合金造形物およびコバルト基合金製造物の製造方法
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CN114054773B (zh) * 2021-11-09 2024-03-22 南京理工大学 析出相非均匀分布的叠层异构铝合金板材的制备方法

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CA3061851A1 (fr) 2020-06-10
CA3061851C (fr) 2022-05-31
AU2018422117A1 (en) 2020-06-25

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