WO2020110326A1 - Poudre ramollie d'alliage à base de ni et procédé de production de ladite poudre ramollie - Google Patents

Poudre ramollie d'alliage à base de ni et procédé de production de ladite poudre ramollie Download PDF

Info

Publication number
WO2020110326A1
WO2020110326A1 PCT/JP2019/003833 JP2019003833W WO2020110326A1 WO 2020110326 A1 WO2020110326 A1 WO 2020110326A1 JP 2019003833 W JP2019003833 W JP 2019003833W WO 2020110326 A1 WO2020110326 A1 WO 2020110326A1
Authority
WO
WIPO (PCT)
Prior art keywords
phase
powder
less
based alloy
mass
Prior art date
Application number
PCT/JP2019/003833
Other languages
English (en)
Japanese (ja)
Inventor
敦夫 太田
今野　晋也
Original Assignee
三菱日立パワーシステムズ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 三菱日立パワーシステムズ株式会社 filed Critical 三菱日立パワーシステムズ株式会社
Priority to CN201980003092.XA priority Critical patent/CN111629852B/zh
Priority to KR1020217002557A priority patent/KR102443966B1/ko
Priority to US16/623,897 priority patent/US20210340644A1/en
Priority to JP2020509554A priority patent/JP6826235B2/ja
Priority to EP19817113.4A priority patent/EP3685942A4/fr
Priority to SG11202012579YA priority patent/SG11202012579YA/en
Publication of WO2020110326A1 publication Critical patent/WO2020110326A1/fr

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
    • 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
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force

Definitions

  • the present invention relates to a technology of a Ni (nickel) base alloy material, and more particularly to a Ni base alloy softening powder which is made of a strong precipitation strengthening Ni base alloy material and is suitable for powder metallurgy technology and a method for producing the softening powder. ..
  • Precipitation-strengthened Ni-based alloy materials are widely used as materials for turbine high-temperature members in order to satisfy various required mechanical properties.
  • strong precipitation strengthened Ni with a high ratio of ⁇ '(gamma prime) phase eg, Ni 3 (Al,Ti) phase
  • a base alloy material for example, a Ni base alloy material that precipitates 30% by volume or more of the ⁇ 'phase is used.
  • precision casting methods have been conventionally used for members such as turbine blades and turbine stationary blades from the viewpoint of creep characteristics.
  • hot forging methods have often been used for turbine disks and combustor members from the viewpoint of tensile properties and fatigue properties.
  • Patent Document 1 Japanese Patent Laid-Open No. 9-302450 discloses a method for producing a Ni-based superalloy article having a controlled grain size from a forging preform, which comprises mixing a ⁇ phase and a ⁇ ′ phase.
  • the superalloy preform was hot die forged at a strain rate of about 0.03 to about 10 per second, and the resulting hot die forging superalloy workpiece was isothermally forged.
  • a supersolvus heat treatment to produce a substantially uniform grain microstructure of approximately ASTM 6-8, and cooling the article from the supersolvus heat treatment temperature.
  • Patent Document 1 it is said that even a Ni-based alloy material having a high ⁇ 'phase volume ratio can be manufactured with a high manufacturing yield without cracking.
  • the technique of Patent Document 1 requires a special manufacturing apparatus and a long work time because the hot forging step of superplastic deformation at a low strain rate and the isothermal forging step thereafter are performed (that is, a long work time is required). , Equipment cost and process cost are high).
  • Patent Document 2 discloses a method for manufacturing a Ni-based alloy softening material composed of a Ni-based alloy having a ⁇ 'phase solid solution temperature of 1050°C or higher, in which the softening treatment is performed in the next step.
  • the first step of hot forging the Ni-based alloy material at a temperature lower than the solid solution temperature of the ⁇ 'phase which is a step performed in a temperature range lower than the melting temperature, and lower than the solid solution temperature of the ⁇ 'phase
  • the technique reported in Patent Document 2 can be said to be an epoch-making technique in that a strong precipitation strengthened Ni-based alloy material can be processed/formed at low cost.
  • the solid content of ⁇ 'phase is In the process of hot forging at a temperature lower than the melting temperature (temperature region where two phases of ⁇ phase and ⁇ 'coexist), a normal forging device (a forging device without a special heating and heat retaining mechanism) was used. In this case, the manufacturing yield is likely to decrease due to the temperature decrease during the forging process (their unwanted precipitation of the ⁇ 'phase).
  • one of the technologies for manufacturing compacts/moldings of difficult-to-process materials at low cost is powder metallurgy technology using metal powder.
  • Patent Document 3 US Pat. No. 5,649,280
  • a fine-grained Ni-base superalloy preform for example, a solidified metal powder preform
  • a heat treatment in a subsequent step to be uniform. Forging so as to give residual strain to form a fine structure with a small grain size, and a long-time subsolvus at a temperature higher than the recrystallization temperature and lower than the ⁇ 'phase solvus temperature for the forged material.
  • Patent Document 3 uses powder metallurgy as a means for refining the particle size of the preform to be forged in order to control the particle size of the final Ni-based superalloy material.
  • powder metallurgy as a means for refining the particle size of the preform to be forged in order to control the particle size of the final Ni-based superalloy material.
  • the strong precipitation strengthened Ni-based alloy material cannot be said to have extremely good moldability/moldability due to the hardness of each powder particle. Therefore, conventionally, when applying a powder metallurgy technique, high temperature and/or high pressure processing was required, and it was difficult to drastically reduce the manufacturing cost of a strong precipitation strengthening Ni-based alloy member. In other words, if there is a Ni-based alloy powder that has high formability/formability and is suitable for powder metallurgy, it is expected that the production cost of strong precipitation strengthened Ni-based alloy members will be dramatically reduced. To be done.
  • Ni-based alloy softening powder has a chemical composition such that the equilibrium precipitation amount at 700° C. of the ⁇ ′ phase that precipitates in the ⁇ phase that is the mother phase is 30% by volume or more and 80% by volume or less, and the average of the softening powder is Particle size is 5 ⁇ m or more 500 ⁇ m or less, the particles of the softening powder is a powder composed of a polycrystalline body of fine crystals of the ⁇ phase, 20% by volume or more of the ⁇ 'phase is deposited on the grain boundaries of the fine crystals of the ⁇ phase that constitute the particles, A Ni-based alloy softening powder, characterized in that the particles have a Vickers hardness at room temperature of 370 Hv or less.
  • the chemical composition is 5 mass% or more and 25 mass% or less of Cr (chrome), 0 mass% to 30 mass% or less of Co (cobalt), and 1 mass% or more and 8 mass% or less of Al (aluminum). ), and a total of 1% by mass or more and 10% by mass or less of Ti (titanium), Nb (niobium) and Ta (tantalum), 10% by mass or less of Fe (iron), and 10% by mass or less of Mo (molybdenum).
  • the chemical composition is such that the solid solution temperature of the ⁇ 'phase is 1100°C or higher.
  • the Ni-based alloy softening powder has a chemical composition such that the equilibrium precipitation amount of the ⁇ ′ phase at 700° C. is 45% by volume or more and 80% by volume or less.
  • the Vickers hardness at room temperature of the particles is 350 Hv or less.
  • Another aspect of the present invention is a method for producing the above Ni-based alloy softening powder,
  • the manufacturing method A precursor powder preparation step of preparing a precursor powder having powder particles having the above chemical composition and composed of a polycrystal of fine crystals of the ⁇ phase,
  • the precursor powder is heated to a temperature not lower than the melting point of the ⁇ phase above the solid solution temperature of the ⁇ ′ phase (in the present invention, referred to as high temperature), and the ⁇ ′ phase is referred to as the ⁇ phase.
  • the powder particles are subjected to a high temperature-slow cooling heat treatment for gradually cooling from the temperature to a temperature lower than the solid solution temperature of the ⁇ ′ phase at a cooling rate of 100° C./h or less.
  • a powder softening high temperature-annealing heat treatment step for producing the Ni-based alloy softening powder in which the ⁇ 'phase is deposited in an amount of 20% by volume or more on the grain boundaries of the fine crystals of the ⁇ phase constituting the A method for producing a softening powder of Ni-based alloy is provided.
  • Yet another aspect of the present invention is a method for producing the above Ni-based alloy softening powder,
  • the manufacturing method A single-phase precursor powder preparation step of preparing a single-phase precursor powder having a chemical composition and powder particles comprising a polycrystal of a single-phase fine crystal of the ⁇ phase, With respect to the single-phase precursor powder, by heating to a temperature lower than the solid solution temperature of 80° C. lower than the solid solution temperature of the ⁇ ′ phase (in the present invention, referred to as sub-high temperature).
  • a sub-high temperature-slow cooling heat treatment for gradually cooling at a cooling rate of 100° C./h or less from the temperature is performed.
  • a powder softening sub-high temperature-slow cooling heat treatment step for producing the Ni-based alloy softening powder in which the ⁇ 'phase is precipitated in an amount of 20% by volume or more, and a method for producing a Ni-based alloy softening powder, To do.
  • Yet another aspect of the present invention is a method for producing the above Ni-based alloy softening powder,
  • the manufacturing method A single-phase precursor powder preparation step of preparing a single-phase precursor powder having a chemical composition and powder particles comprising a polycrystal of a single-phase fine crystal of the ⁇ phase, With respect to the single-phase precursor powder, after heating to a temperature lower than the melting point of the ⁇ phase at a solid solution temperature of the ⁇ 'phase or higher, 100 to a temperature lower than the solid solution temperature of the ⁇ 'phase from the temperature.
  • the ⁇ 'phase is formed on the grain boundaries of the single phase fine crystal of the ⁇ phase constituting the particles of the single phase precursor powder.
  • a powder softening high temperature-annealing heat treatment step for producing the Ni-based alloy softening powder precipitated in an amount of 20% by volume or more.
  • the precursor powder preparing step or the single-phase precursor powder preparing step includes an atomizing element step.
  • the equilibrium precipitation amount of ⁇ ′ phase at 700° C., the solid solution temperature, and the melting point (solidus temperature) of the ⁇ phase are equilibrium determined by thermodynamic calculation based on the chemical composition of the Ni-based alloy material.
  • the amount of precipitation and the temperature can be used.
  • a powder having better moldability/moldability than before which is suitable for powder metallurgy, a Ni-based alloy softening powder and the softening powder
  • a manufacturing method can be provided. Further, by applying powder metallurgy technology using the Ni-based alloy softening powder, it becomes possible to provide a strong precipitation-strengthened Ni-based alloy member with a high production yield (that is, at a lower cost than conventional). ..
  • FIG. 3 is a schematic diagram showing an example of changes in the microstructure of Ni-based alloy powder in the manufacturing method according to the present invention.
  • FIG. 6 is a flow chart showing another example of steps of a method for manufacturing a Ni-based alloy member using the Ni-based alloy softening powder according to the present invention.
  • FIG. 3 is a schematic diagram showing an example of changes in the microstructure of the Ni-based alloy powder in the single-phase precursor powder preparation step-powder softening sub-high temperature-annealing heat treatment step.
  • FIG. 6 is a flow chart showing still another example of the steps of the method for producing a Ni-based alloy member using the Ni-based alloy softening powder according to the present invention.
  • FIG. 1 is a schematic diagram showing a relationship between a ⁇ phase and a ⁇ ′ phase in a precipitation strengthened Ni-based alloy material. (a) When the ⁇ ′ phase is precipitated in the crystal grains of the ⁇ phase, (b) ⁇ This is the case where the ⁇ ′ phase is precipitated on the grain boundaries of the crystal grains of the phase.
  • the atom 1 forming the ⁇ phase and the atom 2 forming the ⁇ ′ phase form the matching interface 3.
  • the ⁇ 'phase precipitates while lattice matching with the ⁇ phase).
  • Such a ⁇ 'phase is referred to as an intragranular ⁇ 'phase (sometimes referred to as a matched ⁇ 'phase).
  • the intragranular ⁇ 'phase is considered to hinder the movement of dislocations within the ⁇ -phase crystal grains because it forms the matching interface 3 with the ⁇ -phase, thereby improving the mechanical strength of the Ni-based alloy material. it is conceivable that.
  • the precipitation-strengthened Ni-based alloy material usually means the state shown in FIG.
  • the atoms forming the ⁇ phase are 1 and the atom 2 forming the ⁇ ′ phase form a non-coherent interface 4 (the ⁇ ′ phase is precipitated in a state not lattice-matched with the ⁇ phase).
  • a ⁇ 'phase is referred to as a grain boundary ⁇ 'phase (may be referred to as an intergranular ⁇ 'phase or an incoherent ⁇ 'phase).
  • the grain boundary ⁇ ′ phase does not hinder the movement of dislocations within the ⁇ phase crystal grain because it forms the non-coherent interface 4 with the ⁇ phase.
  • the grain boundary ⁇ 'phase hardly contributes to the strengthening of the Ni-based alloy material. From these facts, in the Ni-based alloy material, if the grain boundary ⁇ ′ phase is positively deposited instead of the intragranular ⁇ ′ phase, the alloy material becomes in a softened state and the formability is dramatically improved. be able to.
  • the present invention does not precipitate a grain boundary ⁇ ′ phase by performing hot forging in a two-phase coexisting temperature region of ⁇ phase/ ⁇ ′ phase on an alloy lump (ingot) as in Patent Document 2, Forming a precursor powder/single-phase precursor powder of a Ni-based alloy in which powder particles are composed of a polycrystal of ⁇ -phase fine crystals or single-phase fine crystals, and the precursor powder/single-phase precursor powder
  • a major feature of the softening powder is that the grain boundary ⁇ ′ phase is precipitated in an amount of 20% by volume or more on the grain boundaries of the fine crystals of the ⁇ phase constituting the powder particles by subjecting the powder to a predetermined heat treatment. It can be said that the Ni-based alloy precursor powder/single-phase precursor powder is one of the key points.
  • the precipitation of the ⁇ 'phase basically requires the diffusion and rearrangement of the atoms that form the ⁇ 'phase. It is considered that the ⁇ ′ phase preferentially precipitates in the ⁇ phase crystal grains, which requires a short rearrangement distance. Even if it is a cast material, it cannot be denied that the ⁇ 'phase is precipitated on the grain boundaries of the ⁇ -phase crystal.
  • the present inventors have earnestly studied a technique for suppressing the grain growth of ⁇ phase crystal grains even in the vicinity of the solid solution temperature of the ⁇ ′ phase or in the temperature region above the solid solution temperature.
  • the powder particles will be composed of a polycrystalline ⁇ -phase fine crystal (powder particles). It was found that the grain boundaries of the ⁇ -phase fine crystals exist inside the powder particles, which are composed of the ⁇ -phase fine crystals. Furthermore, such powder particles can suppress the grain growth of ⁇ phase fine crystals even if the temperature is raised to around the solid solution temperature of the ⁇ ′ phase or above the solid solution temperature (the powder particles are single crystal bodies of the ⁇ phase). It was found that the grain boundary ⁇ 'phase can be positively precipitated and grown on the grain boundaries of the ⁇ phase fine crystal by maintaining the polycrystal without changing the temperature) and gradually cooling from the temperature. .. The present invention is based on this finding.
  • FIG. 2 is a flow chart showing a process example of a method for manufacturing a Ni-based alloy member using the Ni-based alloy softening powder according to the present invention.
  • the manufacturing method of the Ni-based alloy member using the Ni-based alloy softening powder of the present invention is roughly a polycrystalline body having a predetermined chemical composition and powder particles of ⁇ -phase fine crystals.
  • a precursor powder preparation step (S1) for preparing a precursor powder composed of the above, and a predetermined high temperature-slow cooling heat treatment is applied to the precursor powder to precipitate 20% by volume or more of the grain boundary ⁇ 'phase.
  • the precursor powder preparation step S1 and the powder softening high temperature-slow cooling heat treatment step S2 are the method for producing the Ni-based alloy softening powder according to the present invention.
  • the precursor powder, the powder particles are composed of a polycrystalline ⁇ -phase fine crystals, ⁇ 'phase is not precipitated on the grain boundaries of the ⁇ -phase fine crystals (at least intentionally A powder in a state where the grain boundary ⁇ 'phase is not precipitated).
  • the softening powder refers to a powder in which 20% by volume or more of the grain boundary ⁇ 'phase is precipitated on the grain boundary of the ⁇ phase fine crystal.
  • FIG. 3 is a schematic diagram showing an example of changes in the microstructure of the Ni-based alloy powder in the manufacturing method according to the present invention.
  • the Ni-based alloy precursor powder prepared in the precursor powder preparing step is a powder having an average particle size of 500 ⁇ m or less, and the powder particles are composed of a polycrystal of ⁇ -phase fine crystals. Strictly speaking, it is strongly affected by the temperature history (eg, cooling rate) in the process of forming the precursor powder, but the ⁇ phase (consistent ⁇ ′ phase) is not precipitated in the ⁇ phase fine crystal. The fine crystals and the ⁇ phase fine crystals in which the ⁇ ′ phase in the grains are partially precipitated may coexist.
  • Intragranular ⁇ 'phase is not precipitated ⁇ -phase fine crystals or ⁇ -phase fine crystals in the region where intragranular ⁇ 'phase is not precipitated is the composition before the supersaturated state of ⁇ 'phase or ⁇ 'phase is formed. It is considered to be in a fluctuating state.
  • the particles of the precursor powder are basically composed of a polycrystal of ⁇ -phase fine crystals, but it cannot be ruled out that a part of the particles is composed of a ⁇ -phase single crystal. ..
  • the precursor powder most of the particles are composed of a polycrystal of gamma phase fine crystals, but particles composed of a gamma phase single crystal may be mixed.
  • the precursor powder is heated to a temperature above the solid solution temperature of the ⁇ 'phase and below the melting point of the ⁇ phase.
  • the heating temperature is equal to or higher than the solid solution temperature of the ⁇ 'phase, in terms of thermal equilibrium, all the ⁇ 'phases are solid-dissolved in the ⁇ phase to form the ⁇ phase single phase.
  • a softened powder in which 20% by volume or more of the grain boundary ⁇ ′ phase is precipitated on the grain boundaries of the ⁇ phase fine crystals of the powder particles is obtained. .. Since the softening powder has a sufficiently small amount of precipitation of the intragranular ⁇ 'phase, the mechanism of precipitation strengthening does not act, and the formability/formability is dramatically improved. Since the surface of the powder particle can be regarded as a kind of grain boundary of the ⁇ -phase fine crystal, the ⁇ ′ phase precipitated on the surface of the powder particle is also regarded as the grain boundary ⁇ ′ phase.
  • the softening powder obtained is used to apply a powder metallurgy technique to form a molded body having a desired shape (molding step S3).
  • the softening powder of the present invention has dramatically improved molding processability as compared with the conventional strong precipitation strengthening Ni-based alloy powder, the temperature and/or pressure during the molding process can be kept higher than the conventional one. Can also be lowered. This means that the apparatus cost and/or the process cost can be reduced in the molding process.
  • the formed body having the desired shape is subjected to solution heat treatment in which most of the grain boundary ⁇ 'phase is dissolved in the ⁇ phase (for example, the grain boundary ⁇ 'phase is set to 10% by volume or less).
  • an aging heat treatment for precipitating an intragranular ⁇ 'phase in an amount of 30% by volume or more in the crystal grains of the ⁇ phase is performed (solution treatment-aging heat treatment step S4).
  • solution treatment-aging heat treatment step S4 solution treatment-aging heat treatment step S4
  • a strong precipitation strengthened Ni-based alloy member having a desired shape and being sufficiently precipitation strengthened can be obtained.
  • the ease of the molding process by using the softening powder of the present invention leads to a reduction in the device cost, a reduction in the process cost, and an improvement in the production yield (that is, a reduction in the production cost of the Ni-based alloy member).
  • the obtained strong precipitation strengthened Ni-based alloy member can be suitably used as a next-generation turbine high temperature member (for example, turbine rotor blade, turbine stationary blade, rotor disk, combustor member, boiler member, heat resistant coating material).
  • a next-generation turbine high temperature member for example, turbine rotor blade, turbine stationary blade, rotor disk, combustor member, boiler member, heat resistant coating material.
  • the technique of Patent Document 2 intentionally leaves the coherent ⁇ ′ phase (intragranular ⁇ ′ phase) while precipitating the noncoherent ⁇ ′ phase (grain boundary ⁇ ′ phase, intergranular ⁇ ′ phase). Since a softened body is produced, highly precise control is required. On the other hand, the technique of the present invention produces a softened powder in which the intragranular ⁇ 'phase is once eliminated and then the grain boundary ⁇ 'phase is precipitated.
  • the softened powder can be obtained by the combination of the precursor powder forming step S1 with low industrial difficulty and the powder softening high temperature-slow cooling heat treatment step S2 with low industrial difficulty, it is more versatile than the technique of Patent Document 2. The cost is high and the cost of the entire manufacturing process can be reduced. In particular, it is effective for producing a softened powder made of a super strong precipitation strengthened Ni-based alloy material having a volume ratio of ⁇ 'phase of 45% by volume or more.
  • This step S1 is a step of preparing a Ni-based alloy precursor powder having a predetermined chemical composition (in particular, intentionally containing a predetermined amount of oxygen component).
  • a method/method for preparing the precursor powder basically the conventional method/method can be used.
  • the atomizing element process (S1b) is performed.
  • a classifier step (S1c) for making the particle size of the precursor powder uniform may be performed.
  • the oxygen content in the atomizing element process S1b It is preferable to control the oxygen content in the atomizing element process S1b.
  • the conventional method/method can be used except that the oxygen content in the Ni-based alloy is controlled.
  • a gas atomizing method or a centrifugal atomizing method while controlling the oxygen amount (oxygen partial pressure) in the atomizing atmosphere can be preferably used.
  • the content of the oxygen component in the precursor powder (sometimes referred to as the content rate) is preferably 0.003 mass% (30 ppm) or more and 0.05 mass% (500 ppm) or less, more preferably 0.005 mass% or more and 0.04 mass% or less. , More preferably 0.007 mass% or more and 0.02 mass% or less. If it is less than 0.003 mass %, the effect of suppressing the grain growth of ⁇ -phase fine crystals is small, and if it exceeds 0.05 mass %, the mechanical strength and ductility of the final Ni-based alloy member are reduced. It is considered that the oxygen atoms form a solid solution inside the powder particles or generate nuclei of oxide on the surface or inside.
  • the chemical composition of the Ni-based alloy one in which the ⁇ 'phase solid solution temperature is 1020°C or higher. It is more preferable to use a material having a temperature of 1050° C. or higher, and it is more preferable to use a material having a temperature of 1100° C. or higher. Details of the chemical composition other than oxygen components will be described later.
  • the average particle size of the precursor powder is preferably 5 ⁇ m or more and 500 ⁇ m or less, more preferably 10 ⁇ m or more and 300 ⁇ m or less, still more preferably 20 ⁇ m or more and 200 ⁇ m or less.
  • the average particle size of the precursor powder can be measured using, for example, a laser diffraction type particle size distribution measuring device.
  • the particles of the precursor powder basically consist of a polycrystalline body of ⁇ -phase fine crystals, and the average grain size of the ⁇ -phase fine crystals in the powder particles is 5 ⁇ m or more and 50 ⁇ m or less. Is preferred.
  • the ⁇ 'phase for example, a eutectic ⁇ 'phase that directly crystallizes from the liquid phase
  • the ⁇ 'phase precipitates on the grain boundaries of the ⁇ phase fine crystals. do not do.
  • step S2 the precursor powder prepared in the previous step S1 is heated to a temperature equal to or higher than the solid solution temperature of the ⁇ ′ phase to once dissolve the ⁇ ′ phase in the ⁇ phase, and then from the temperature. It is a step of producing a softened powder by generating and increasing the grain boundary ⁇ ′ phase by slow cooling.
  • the slow cooling start temperature is preferably lower than the melting point of the ⁇ -phase (below the solidus temperature) and 35°C higher than the solid-solution temperature of the ⁇ 'phase.
  • the temperature is preferably higher than or equal to the high temperature, and more preferably 25° C. or higher than the solid solution temperature of the ⁇ ′ phase.
  • the melting point of the ⁇ phase is lower than the “solid solution temperature of the ⁇ ′ phase +35°C” or the “solid solution temperature of the ⁇ ′ phase +25°C”, the “less than the melting point of the ⁇ phase” naturally takes precedence. ..
  • the heat treatment atmosphere is a non-oxidizing atmosphere (an atmosphere containing no partial pressure of oxygen that causes oxidation) to prevent undesired oxidation of the Ni-based alloy powder (oxidation exceeding the oxygen content controlled in the previous step S1). If there is no particular limitation, a reducing atmosphere (for example, hydrogen gas atmosphere) is more preferable.
  • the intragranular ⁇ 'phase does not completely disappear as a result of the high temperature-slow cooling heat treatment, and that it exists only slightly.
  • the grain boundary ⁇ ′ phase is precipitated in an amount of 20% by volume or more
  • the amount of the intragranular ⁇ ′ phase is 10% by volume or less
  • the molding processability in the subsequent molding process step is strongly hindered. It is acceptable because it does not.
  • the amount of the intragranular ⁇ 'phase present is more preferably 5% by volume or less, further preferably 3% by volume or less.
  • the precursor powder prepared in the precursor powder preparing step S1 contains more oxygen component as the alloy composition than the conventional Ni-based alloy material (see that it contains a large amount of oxygen component. Controlled by). Then, when such a precursor powder is subjected to a heat treatment at a solid solution temperature of the ⁇ 'phase or higher, it is considered that the contained oxygen atoms combine with the metal atoms of the alloy to form a local oxide.
  • the oxide formed at this time suppresses the grain boundary migration of ⁇ -phase fine crystals (that is, grain growth of ⁇ -phase fine crystals). That is, it is considered that even if the ⁇ 'phase disappears in this step S2, the coarsening of the ⁇ phase fine crystals can be prevented.
  • the strengthening mechanism of the precipitation strengthened Ni-based alloy material is that it contributes to strengthening by forming a coherent interface between the ⁇ phase and the ⁇ ′ phase, and the non-coherent interface does not contribute to strengthening.
  • the amount of intragranular ⁇ 'phase (coherent ⁇ 'phase) and increasing the amount of grain boundary ⁇ 'phase (intergranular ⁇ 'phase, non-coherent ⁇ 'phase) it has excellent moldability. A softened powder can be obtained.
  • ⁇ Lower cooling rate in the slow cooling process is more advantageous for precipitation and growth of grain boundary ⁇ 'phase.
  • the cooling rate is preferably 100° C./h or less, more preferably 50° C./h or less, even more preferably 10° C./h or less. If the cooling rate is higher than 100° C./h, the intragranular ⁇ ′ phase is preferentially precipitated and the effect of the present invention cannot be sufficiently obtained.
  • the precipitation amount of the intragranular ⁇ 'phase is preferably 10% by volume or less, and more preferably 5% by volume or less.
  • the precipitation amount of the ⁇ ′ phase can be measured by microstructural observation and image analysis (for example, ImageJ, public domain software developed by National Institutes of Health in the US).
  • the end temperature of the slow cooling process when the ⁇ 'phase solid solution temperature is relatively low 1020 °C or more and less than 1100 °C, a temperature lower than the ⁇ 'phase solid solution temperature by 50 °C or more is preferable, and the ⁇ 'phase solid solution A temperature lower than the temperature by 100° C. or more is more preferable, and a temperature lower than the ⁇ ′ phase solid solution temperature by 150° C. or more is further preferable.
  • the end temperature of the slow cooling process is preferably 100°C or more lower than the ⁇ 'phase solid solution temperature, and 150°C from the ⁇ 'phase solid solution temperature.
  • the lower temperature is more preferable, and the temperature lower than the ⁇ 'phase solid solution temperature by 200°C or more is further preferable. More specifically, it is preferable to gradually cool to a temperature of 1000°C or lower and 800°C or higher.
  • a higher cooling rate is preferable in order to suppress precipitation of the intragranular ⁇ 'phase during cooling (for example, to set the precipitation amount of the intragranular ⁇ 'phase to 10% by volume or less).
  • water cooling or gas cooling is preferable.
  • the Vickers hardness (Hv) of the softened powder at room temperature can be used as an index of moldability/moldability.
  • the softened powder obtained by performing this step S2 has a room temperature Vickers hardness even if it is a super strong precipitation strengthening Ni-based alloy material such that the equilibrium precipitation amount of the ⁇ 'phase at 700°C is 45% by volume or more. You can get less than 370 Hv.
  • the room temperature Vickers hardness is more preferably 350 Hv or less, and further preferably 330 Hv or less.
  • FIG. 4 is a flow chart showing another example of steps of the method for manufacturing a Ni-based alloy member using the Ni-based alloy softening powder according to the present invention.
  • another manufacturing method of the Ni-based alloy softening powder using the Ni-based alloy softening powder of the present invention is a manufacturing method of the Ni-based alloy softening powder (single-phase precursor powder preparation step S1′ and powder In the softening sub-high temperature-slow cooling heat treatment step S2'), unlike the step of FIG. 2, the forming step S3 and the solution-aging heat treatment step S4 are the same as those of FIG.
  • FIG. 5 is a schematic diagram showing an example of changes in the microstructure of the Ni-based alloy powder in steps S1' and S2'.
  • steps S1′ to S2′ that is, the other method for producing the Ni-based alloy softening powder according to the present invention
  • steps S1′ to S2′ that is, the other method for producing the Ni-based alloy softening powder according to the present invention
  • This step S1′ is a step of preparing a single-phase precursor powder having a predetermined chemical composition and powder particles composed of a single-phase microcrystalline polycrystal of ⁇ phase.
  • the single-phase precursor powder means a ⁇ -phase single-phase ( ⁇ ′) measured by a scanning electron microscope-energy dispersive X-ray analyzer (SEM-EDX) and/or an X-ray diffractometer (XRD). It means a powder that can be judged to have no phase detected). It does not require strictness at the level of transmission electron microscope (TEM) or scanning transmission electron microscope (STEM).
  • This step S1' includes a mother alloy ingot producing element step (S1a) similar to step S1, and an atomizing element step (S1'b) for forming a single-phase precursor powder, and if necessary, the step The classifier step (S1c) similar to S1 may be performed.
  • the atomizing element step S1'b is the same atomizing method as the atomizing element step S1b of step S1 except that the average cooling rate in the temperature range where the ⁇ 'phase is easily generated and precipitated (eg, 1100°C to 600°C) is controlled. Is available.
  • the average cooling rate to be controlled is preferably 500° C./min or higher, more preferably 1000° C./min or higher, further preferably 1500° C./min or higher, most preferably 2000° C./min or higher.
  • step S1' a single-phase precursor powder composed of a single-phase fine-crystal polycrystal of the ⁇ phase is obtained as shown in FIG.
  • the content of the oxygen component in the single-phase precursor powder, the average grain size, and the average crystal grain size of the single-phase fine crystals are the same as those of the precursor powder obtained in step S1.
  • step S2' is a Ni-based alloy in which 20 volume% or more of the grain boundary ⁇ 'phase is precipitated by subjecting the single-phase precursor powder prepared in the previous step S1' to a predetermined sub-high temperature-annealing heat treatment.
  • This is a step of producing a softened powder.
  • Sub-high temperature-slow cooling heat treatment is heating at a temperature 80°C lower than the solid solution temperature of the ⁇ 'phase to a temperature lower than the solid solution temperature, and then gradually cooled from that temperature at a cooling rate of 100°C/h or less. Heat treatment.
  • the heating temperature (that is, the gradual cooling start temperature) is more preferably 50° C.
  • the cooling rate in the slow cooling process is preferably 50° C./h or less, more preferably 10° C./h or less.
  • the grain boundary ⁇ 'phase preferentially nucleates and grows even when the slow cooling start temperature is in the sub-high temperature range (see Fig. 5). Further, regarding the gradual cooling end temperature in step S2′, the cooling from the gradual cooling end temperature, the precipitation amount of the grain boundary ⁇ ′ phase and the existing amount of the intragranular ⁇ ′ phase as a result of the sub-high temperature-gradual cooling heat treatment, It is similar to those of the softened powder obtained in S2.
  • the softened powder similar to the softened powder obtained in step S2 can be obtained by the sub-high temperature-slow cooling heat treatment for the single-phase precursor powder.
  • the exact mechanism has not been clarified at this stage, but it is possible that the single-phase precursor powder composed of a single-phase microcrystalline polycrystal of the ⁇ phase is an important point. Can be considered.
  • a temperature of 80° C. or more lower than the solid solution temperature of the ⁇ ′ phase and lower than the solid solution temperature (in the present invention, a sub-high temperature) Is considered to be a temperature range in which the degree of supercooling associated with the precipitation of the ⁇ 'phase is small.
  • Precipitation of the ⁇ 'phase (that is, intragranular ⁇ 'phase) in the ⁇ -phase crystal is considered to be a kind of homogeneous nucleation (at least a phenomenon similar to homogeneous nucleation).
  • the nucleation frequency of the intragranular ⁇ 'phase in the sub-high temperature region in the ⁇ -phase single-phase crystal is considered to be very low.
  • the sub-high temperature-slow cooling heat treatment for the single-phase precursor powder is performed by competing the homogeneous nucleation and the heterogeneous nucleation in the temperature region where the degree of supercooling of the ⁇ ′ phase is small, It is considered that the heat treatment is carried out by preferentially nucleating the grain boundary ⁇ 'phase due to the heterogeneous nucleation, and then grain-growing the nuclei generated in the slow cooling process.
  • the consideration (model) is considered to be applicable to "preferential nucleation of grain boundary ⁇ 'phase and subsequent grain growth of grain boundary ⁇ 'phase" in the powder softening high temperature-slow cooling heat treatment step S2.
  • FIG. 6 is a flow chart showing still another process example of the method for producing a Ni-based alloy member using the Ni-based alloy softening powder according to the present invention.
  • the manufacturing method of the Ni-based alloy member using the Ni-based alloy softening powder of the present invention is, in the production of the Ni-based alloy softening powder, after the single-phase precursor powder preparing step S1′.
  • the powder softening high temperature-slow cooling heat treatment step S2 is performed.
  • the forming step S3 and the solution heat treatment-aging heat treatment step S4 may be the same as those in FIG.
  • the chemical composition of the Ni-based alloy material used in the present invention will be described.
  • the Ni-based alloy material has a chemical composition such that the equilibrium precipitation amount of the ⁇ ′ phase at 700° C. is 30% by volume or more and 80% by volume or less. Specifically, in mass%, 5% or more and 25% or less of Cr, 0% or more and 30% or less of Co, 1% or more and 8% or less of Al, and the sum of Ti, Nb, and Ta is 1% or more and 10% or less.
  • the Cr component dissolves in the ⁇ phase and has the effect of improving the corrosion resistance and oxidation resistance by forming an oxide film (Cr 2 O 3 ) on the surface under the actual use environment of the Ni-based alloy material. ..
  • an oxide film Cr 2 O 3
  • excessive addition promotes the formation of a harmful phase, it is preferably 25% by mass or less.
  • the Co component is an element close to Ni and forms a solid solution in the ⁇ phase in the form of substitution with Ni, and has the effect of improving creep strength and corrosion resistance. Further, it also has the effect of lowering the solid solution temperature of the ⁇ 'phase, and improves the high temperature ductility. However, excessive addition promotes the formation of a harmful phase, so the content is preferably more than 0% and 30% by mass or less.
  • the Al component is an essential component for forming the ⁇ 'phase which is the precipitation strengthening phase of the Ni-based alloy. Furthermore, by forming an oxide film (Al 2 O 3 ) on the surface of the Ni-based alloy material in the actual use environment, it contributes to the improvement of oxidation resistance and corrosion resistance.
  • the amount is preferably 1% by mass or more and 8% by mass or less depending on the desired amount of ⁇ 'phase precipitation.
  • Ti component, Nb component and Ta component have the effect of forming ⁇ 'phase and improving high temperature strength like Al component. Further, the Ti component and the Nb component also have the effect of improving the corrosion resistance. However, since excessive addition promotes the formation of a harmful phase, it is preferable that the total amount of Ti, Nb, and Ta components is 1% by mass or more and 10% by mass or less.
  • the Mo component and W component have the effect of forming a solid solution in the ⁇ phase to improve the high temperature strength (solid solution strengthening), and it is preferable to add at least one of them.
  • the Mo component also has the effect of improving corrosion resistance.
  • the Mo component is 10 mass% or less and the W component is 8 mass% or less.
  • Zr component, B component, and C component strengthen the ⁇ -phase grain boundaries (strengthen the tensile strength in the direction perpendicular to the ⁇ -phase grain boundaries) and improve the high temperature ductility and creep strength. There is. However, since excessive addition deteriorates moldability, it is preferable that the Zr component is 0.1 mass% or less, B is 0.1 mass% or less, and C is 0.2 mass% or less.
  • the Hf component has the effect of improving oxidation resistance. However, since excessive addition promotes the formation of a harmful phase, it is preferable to set the content to 2% by mass or less.
  • Re component contributes to the solid solution strengthening of ⁇ phase and also has the effect of contributing to the improvement of corrosion resistance. However, excessive addition promotes the formation of harmful phases. In addition, since Re is an expensive element, increasing the amount of addition has the demerit of increasing the material cost of the alloy. Therefore, Re is preferably 5% by mass or less.
  • the O component is usually treated as an impurity and is a component to be reduced as much as possible, but in the present invention, as described above, the grain growth of the ⁇ phase fine crystal is suppressed and the formation of grain boundary ⁇ ′ phase grains is suppressed. It is an essential ingredient for promotion.
  • the O content is preferably 0.003 mass% or more and 0.05 mass% or less.
  • Residual components of the Ni-based alloy material become unavoidable impurities other than Ni and O components.
  • unavoidable impurities other than the O component include N (nitrogen), P (phosphorus), and S (sulfur).
  • Example 1 (Preparation of Ni-based alloy precursor powders PP1 to PP8 and single-phase precursor powders PP9 to PP10)
  • a master ingot (10 kg) was prepared by mixing, melting, and casting the Ni-based alloy raw materials. The dissolution was performed by the vacuum induction heating dissolution method. Next, the obtained master ingot was redissolved and a Ni-based alloy powder was produced by the gas atomizing method while controlling the oxygen partial pressure in the atomizing atmosphere.
  • Ni-based alloy powder is classified to select alloy powders having a particle size in the range of 25 to 150 ⁇ m, and Ni-based alloy precursor powders PP1 to PP8 and single-phase precursor powders PP9 to PP10 are prepared. .. Table 1 shows the chemical compositions of the obtained powders PP1 to PP10.
  • Example 2 (Production of Ni-based alloy softening powders of Examples 1 to 11 and Comparative Examples 1 to 12 and evaluation of molding processability)
  • the precursor powders PP1 to PP8 and the single-phase precursor powders PP9 to PP10 obtained in Experiment 1 were softened under the heat treatment conditions (slow cooling start temperature, slow cooling process cooling rate) shown in Table 2 below.
  • the Ni-based alloy softening powders of Examples 1 to 11 and Comparative Examples 1 to 12 were produced.
  • the end temperature of the slow cooling process was 950° C. except for Comparative Examples 1 and 12.
  • gas was rapidly cooled from the slow cooling start temperature to room temperature.
  • the precipitation amount of the grain boundary ⁇ 'phase was determined by observing the softened powder with an electron microscope and image analysis (ImageJ).
  • the room temperature Vickers hardness of the softened powder was measured by randomly extracting 10 particles and using a micro Vickers hardness meter (Akashi Seisakusho, Model: MVK-E). Of the 10 particles at room temperature Vickers hardness, the average value of the room temperature Vickers hardness of 8 particles excluding the maximum value and the minimum value was defined as the room temperature Vickers hardness of the softened powder. In the moldability evaluation, a room temperature Vickers hardness of 370 Hv or less was judged as "pass", and a room temperature Vickers hardness of more than 370 Hv was judged as "fail”.
  • Table 2 shows specifications and evaluation results of the Ni-based alloy softening powders of Examples 1 to 11 and Comparative Examples 1 to 12.
  • Table 2 shows specifications and evaluation results of the Ni-based alloy softening powders of Examples 1 to 11 and Comparative Examples 1 to 12.
  • the equilibrium precipitation amount and the solid solution temperature of the ⁇ 'phase at 700°C of the ⁇ 'phase are obtained from the alloy composition of Table 1 based on thermodynamic calculation.
  • the softening powders of Comparative Examples 1 to 7 in which the starting temperature and/or the cooling rate of the slow cooling process in the high temperature-slow cooling heat treatment were out of the range of the present invention were the precipitation amount of the grain boundary ⁇ 'phase. Is less than 20% by volume (instead, an increase in the amount of ⁇ 'phase precipitation in grains is confirmed), and the room temperature Vickers hardness is more than 370 Hv. As a result, the moldability was judged to be unacceptable. If the slow cooling start temperature (that is, the heating temperature) in the high temperature-slow cooling heat treatment is too low, or if the cooling rate in the slow cooling process is too high, the grain boundary ⁇ 'phase hardly precipitates and grows. It was confirmed that the sex could not be secured.
  • the softened powder of Comparative Example 8 in which the equilibrium precipitation amount of the ⁇ 'phase at 700°C deviates from the definition of the present invention, the softening powder of Comparative Example 8 has an equilibrium precipitation amount of the ⁇ 'phase of less than 30% by volume. It does not apply to the targeted strong precipitation strengthened Ni-based alloy materials. However, since the amount of ⁇ 'phase precipitation is absolutely small, there has been no particular problem in molding processability/molding processability.
  • the softened powders of Examples 8 to 9 using the single-phase precursor powders PP9 to PP10 have a grain size even if they are subjected to the sub-high temperature-annealing heat treatment in which the annealing start temperature is lower than the solid solution temperature of the ⁇ 'phase.
  • the precipitation amount of the boundary ⁇ 'phase is 20% by volume or more, and the room temperature Vickers hardness is 370 Hv or less. As a result, the moldability was judged to be acceptable. That is, the effect of the present invention was confirmed.
  • the softened powders of Examples 10 to 11 in which the high temperature-slow cooling heat treatment was applied to the single-phase precursor powders PP9 to PP10 also had the precipitation amount of the grain boundary ⁇ 'phase of 20% by volume or more, and the room temperature Vickers hardness. Is less than 370 Hv. As a result, the moldability was judged to be acceptable. That is, the effect of the present invention was confirmed.
  • the softening powders of Comparative Examples 9 to 12 in which the starting temperature or the cooling rate of the slow cooling process in the softening process did not satisfy the requirements of the present invention the precipitation of the grain boundary ⁇ 'phase was observed.
  • the amount is less than 20% by volume, and the room temperature Vickers hardness is more than 370 Hv.
  • the moldability was judged to be unacceptable. If the slow cooling start temperature in the sub-high temperature-slow cooling heat treatment is too low, or if the cooling rate in the slow cooling process in the high temperature-slow cooling heat treatment is too high, the grain boundary ⁇ 'phase hardly precipitates and grows, resulting in sufficient molding. It was confirmed that the workability could not be secured.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

La présente invention aborde le problème de fourniture : d'une poudre ramollie d'alliage à base de Ni qui est une poudre présentant une meilleure aptitude au façonnage/moulage que précédemment en dépit du fait que la poudre soit produite à l'aide d'un matériau d'alliage à base de Ni durci fortement par précipitation et qui est appropriée pour une technique de métallurgie des poudres ; et d'un procédé de production de la poudre ramollie. La poudre ramollie d'alliage à base de Ni selon la présente invention est une poudre qui présente une composition chimique telle que la quantité de précipitation à l'équilibre d'une phase γ' précipitée dans une phase γ qui sert de phase de matrice représente 30 à 80 % en volume à 700 °C et présente une grosseur moyenne de grain de 5 à 500 µm, chacun des grains de la poudre ramollie étant formé d'un corps polycristallin de microcristaux de la phase γ, la poudre étant caractérisée en ce que la phase γ' est précipitée en une quantité de 20 % en volume ou plus sur les limites de grain des microcristaux de la phase γ qui constituent les grains et la dureté Vickers des grains à température ambiante est inférieure ou égale à 370 Hv.
PCT/JP2019/003833 2018-11-30 2019-02-04 Poudre ramollie d'alliage à base de ni et procédé de production de ladite poudre ramollie WO2020110326A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
CN201980003092.XA CN111629852B (zh) 2018-11-30 2019-02-04 Ni基合金软化粉末和该软化粉末的制造方法
KR1020217002557A KR102443966B1 (ko) 2018-11-30 2019-02-04 Ni기 합금 연화 분말 및 해당 연화 분말의 제조 방법
US16/623,897 US20210340644A1 (en) 2018-11-30 2019-02-04 Ni-Based Alloy Softened Powder and Method for Manufacturing Same
JP2020509554A JP6826235B2 (ja) 2018-11-30 2019-02-04 Ｎｉ基合金軟化粉末および該軟化粉末の製造方法
EP19817113.4A EP3685942A4 (fr) 2018-11-30 2019-02-04 Poudre ramollie d'alliage à base de ni et procédé de production de ladite poudre ramollie
SG11202012579YA SG11202012579YA (en) 2018-11-30 2019-02-04 Ni-BASED ALLOY SOFTENED POWDER AND METHOD FOR MANUFACTURING SAME

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2018-224833 2018-11-30
JP2018224833 2018-11-30

Publications (1)

Publication Number Publication Date
WO2020110326A1 true WO2020110326A1 (fr) 2020-06-04

Family

ID=70851954

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2019/003833 WO2020110326A1 (fr) 2018-11-30 2019-02-04 Poudre ramollie d'alliage à base de ni et procédé de production de ladite poudre ramollie

Country Status (7)

Country Link
US (1) US20210340644A1 (fr)
EP (1) EP3685942A4 (fr)
JP (1) JP6826235B2 (fr)
KR (1) KR102443966B1 (fr)
CN (1) CN111629852B (fr)
SG (1) SG11202012579YA (fr)
WO (1) WO2020110326A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023027054A1 (fr) * 2021-08-27 2023-03-02 国立研究開発法人物質・材料研究機構 Superalliage à base de nickel et poudre associée, et procédé de fabrication d'un article moulé en superalliage à base de nickel

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112281099A (zh) * 2020-10-13 2021-01-29 江苏联捷冶金设备有限公司 钨钴合金沉没辊及其制备方法
EP4001445A1 (fr) * 2020-11-18 2022-05-25 Siemens Energy Global GmbH & Co. KG Superalliage a base de nickel ayant une résistance à l'oxydation élevée et une bonne aptitude au traitement
DE102021204745A1 (de) * 2021-05-11 2022-11-17 Siemens Energy Global GmbH & Co. KG Legierung, Pulver, Verfahren und Bauteil
CN115233074A (zh) * 2022-07-12 2022-10-25 北京科技大学 一种燃机动叶片用钴镍基高温合金及其制备方法
CN116043066B (zh) * 2022-12-21 2024-05-03 东方电气集团东方汽轮机有限公司 一种低扩散性活化辅助剂及其应用、修复剂及其制备、合金修复方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5061324A (en) * 1990-04-02 1991-10-29 General Electric Company Thermomechanical processing for fatigue-resistant nickel based superalloys
US5649280A (en) 1996-01-02 1997-07-15 General Electric Company Method for controlling grain size in Ni-base superalloys
JPH09302450A (ja) 1996-02-07 1997-11-25 General Electric Co <Ge> ニッケル基超合金における結晶粒度の制御
JP2016003374A (ja) * 2014-06-18 2016-01-12 三菱日立パワーシステムズ株式会社 Ｎｉ基合金軟化材及びＮｉ基合金部材の製造方法
WO2016053489A2 (fr) * 2014-08-18 2016-04-07 General Electric Company Superalliages améliorés par l'ajout de zirconium

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8992699B2 (en) * 2009-05-29 2015-03-31 General Electric Company Nickel-base superalloys and components formed thereof
US20100329876A1 (en) * 2009-06-30 2010-12-30 General Electric Company Nickel-base superalloys and components formed thereof
EP2591135B1 (fr) 2010-07-09 2015-09-09 General Electric Company Alliage à base de nickel, son traitement et les composants formés à partir dudit alliage
CN105189794B (zh) * 2013-07-17 2017-11-14 三菱日立电力系统株式会社 Ni基合金制品及其制造方法和Ni基合金构件及其制造方法
EP2949768B1 (fr) * 2014-05-28 2019-07-17 Ansaldo Energia IP UK Limited Précipitation gamma prime renforcée par un superalliage à base de nickel destinée à être utilisée dans un processus de fabrication d'additif à base de poudre
EP3278901B1 (fr) * 2015-03-30 2020-07-22 Hitachi Metals, Ltd. Procédé de fabrication d'un superalliage à base de ni et résistant à la chaleur
CN113122789B (zh) * 2016-11-16 2022-07-08 三菱重工业株式会社 镍基合金模具和该模具的修补方法
JP6809169B2 (ja) * 2016-11-28 2021-01-06 大同特殊鋼株式会社 Ｎｉ基超合金素材の製造方法
JP6931545B2 (ja) * 2017-03-29 2021-09-08 三菱重工業株式会社 Ｎｉ基合金積層造形体の熱処理方法、Ｎｉ基合金積層造形体の製造方法、積層造形体用Ｎｉ基合金粉末、およびＮｉ基合金積層造形体
WO2018216067A1 (fr) * 2017-05-22 2018-11-29 川崎重工業株式会社 Composant à haute température et procédé de production associé
CN108396269B (zh) * 2018-03-02 2019-11-08 河北工业大学 一种增强多晶Ni3Al基高温合金变形稳定性的热处理方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5061324A (en) * 1990-04-02 1991-10-29 General Electric Company Thermomechanical processing for fatigue-resistant nickel based superalloys
US5649280A (en) 1996-01-02 1997-07-15 General Electric Company Method for controlling grain size in Ni-base superalloys
JPH09302450A (ja) 1996-02-07 1997-11-25 General Electric Co <Ge> ニッケル基超合金における結晶粒度の制御
JP2016003374A (ja) * 2014-06-18 2016-01-12 三菱日立パワーシステムズ株式会社 Ｎｉ基合金軟化材及びＮｉ基合金部材の製造方法
JP5869624B2 (ja) 2014-06-18 2016-02-24 三菱日立パワーシステムズ株式会社 Ｎｉ基合金軟化材及びＮｉ基合金部材の製造方法
WO2016053489A2 (fr) * 2014-08-18 2016-04-07 General Electric Company Superalliages améliorés par l'ajout de zirconium
CN106661675A (zh) * 2014-08-18 2017-05-10 通用电气公司 通过锆添加剂增强的超级合金
JP2017532440A (ja) * 2014-08-18 2017-11-02 ゼネラル・エレクトリック・カンパニイ ジルコニウム添加による強化超合金

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP3685942A4

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023027054A1 (fr) * 2021-08-27 2023-03-02 国立研究開発法人物質・材料研究機構 Superalliage à base de nickel et poudre associée, et procédé de fabrication d'un article moulé en superalliage à base de nickel

Also Published As

Publication number Publication date
EP3685942A1 (fr) 2020-07-29
JP6826235B2 (ja) 2021-02-03
US20210340644A1 (en) 2021-11-04
EP3685942A4 (fr) 2021-03-24
JPWO2020110326A1 (ja) 2021-02-15
KR20210024119A (ko) 2021-03-04
KR102443966B1 (ko) 2022-09-19
CN111629852B (zh) 2023-03-31
SG11202012579YA (en) 2021-06-29
CN111629852A (zh) 2020-09-04

Similar Documents

Publication Publication Date Title
JP6793689B2 (ja) Ｎｉ基合金部材の製造方法
WO2020110326A1 (fr) Poudre ramollie d&#39;alliage à base de ni et procédé de production de ladite poudre ramollie
JP5696995B2 (ja) 耐熱超合金
JP7012468B2 (ja) 超合金物品及び関連物品の製造方法
KR102193336B1 (ko) Ni기 단조 합금재 및 그것을 사용한 터빈 고온 부재
JP6965364B2 (ja) 析出硬化型コバルト−ニッケル基超合金およびそれから製造された物品
JP7073051B2 (ja) 超合金物品及び関連物品の製造方法
WO2016152985A1 (fr) ALLIAGE À BASE DE Ni ULTRA RÉSISTANT À LA CHALEUR ET DISQUE DE TURBINE UTILISANT CELUI-CI
JP5645054B2 (ja) アニーリングツインを含有するニッケル基耐熱超合金と耐熱超合金部材
JP7324254B2 (ja) Ｃｏ基合金材料、Ｃｏ基合金製造物、および該製造物の製造方法
JP2021172851A (ja) Ｎｉ基合金部材の製造方法
JP2012107269A (ja) ニッケル基耐熱超合金と耐熱超合金部材

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2020509554

Country of ref document: JP

Kind code of ref document: A

ENP Entry into the national phase

Ref document number: 2019817113

Country of ref document: EP

Effective date: 20191218

ENP Entry into the national phase

Ref document number: 20217002557

Country of ref document: KR

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE