WO2023100920A1 - 酸化物ナノ粒子を含む積層造形用合金粉末材料および積層造形体 - Google Patents

酸化物ナノ粒子を含む積層造形用合金粉末材料および積層造形体 Download PDF

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Publication number
WO2023100920A1
WO2023100920A1 PCT/JP2022/044113 JP2022044113W WO2023100920A1 WO 2023100920 A1 WO2023100920 A1 WO 2023100920A1 JP 2022044113 W JP2022044113 W JP 2022044113W WO 2023100920 A1 WO2023100920 A1 WO 2023100920A1
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Prior art keywords
alloy powder
mass
oxide nanoparticles
additive manufacturing
powder
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PCT/JP2022/044113
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English (en)
French (fr)
Japanese (ja)
Inventor
透 萩谷
裕樹 池田
芳和 相川
裕樹 森口
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Sanyo Special Steel Co Ltd
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Sanyo Special Steel Co Ltd
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Priority to EP22901352.9A priority Critical patent/EP4442389A4/en
Priority to CN202280077848.7A priority patent/CN118302264A/zh
Priority to US18/715,352 priority patent/US20250018467A1/en
Publication of WO2023100920A1 publication Critical patent/WO2023100920A1/ja
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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
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • 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
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • 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
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/059—Making alloys comprising less than 5% by weight of dispersed reinforcing phases
    • 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
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0261—Matrix based on Fe for ODS steels
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/20—Ferrous alloys, e.g. steel alloys containing chromium with copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/25—Oxide
    • 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
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • 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
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • 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 provides an alloy powder material for additive manufacturing containing particles made of an oxide having a size of nanometers (hereinafter referred to as "oxide nanoparticles”), and an additive model produced by additive manufacturing using the alloy powder material. Regarding.
  • a method of manufacturing a three-dimensional shaped body by irradiating a powder material with a laser beam or an electron beam (hereinafter referred to as a powder sintering lamination method) is known.
  • a powder layer made of metal powder is irradiated with a light beam to form a sintered layer, and the sintered layers are stacked to obtain a three-dimensional shaped body
  • Typical metal additive manufacturing methods include a powder bed method (powder bed fusion method) and a metal deposition method (directed energy deposition method).
  • the modeling layers are stacked by repeating the process of supplying molten powder to a predetermined position and solidifying it to form a modeling layer.
  • the melted powder can be obtained by directly melting the flying powder that is sprayed toward the base material or adhering to the surface of the base material with a laser beam, or indirectly by injecting the powder onto the surface of the base material that has been melted. It is formed by melting into
  • the irradiated parts of the spread powder are melted and solidified by irradiation with a laser beam or an electron beam. This melting and solidification binds the powder particles together.
  • the irradiation is selectively applied to a portion of the metal powder, the non-irradiated portion does not melt, and a bonding layer is formed only on the irradiated portion.
  • New metal powder is spread over the formed bonding layer, and the metal powder is irradiated with a laser beam or an electron beam. The irradiation then melts and solidifies the metal particles to form a new bonding layer.
  • the new tie layer is also bonded to the existing tie layer.
  • a powder obtained by mixing iron-based powder and one or more powders selected from the group consisting of nickel, nickel-based alloys, copper, copper-based alloys, and graphite is used as a metal light.
  • a powder layer forming step of forming a powder layer using metal powder for modeling, a sintered layer forming step of irradiating the powder layer with a beam to form a sintered layer, and a removing step of cutting the surface of the modeled body are repeated.
  • a method has been proposed in which a sintered layer is formed by a method of manufacturing a three-dimensional shaped body (see Patent Document 1).
  • the fluidity of the powder is important in order to spread the powder with high filling properties.
  • the most well-known method for increasing the fluidity of such powder is to increase the circularity of the powder.
  • nanoparticle aggregation part a powder material that does not contain a part where nanoparticles are aggregated
  • a metal powder with a high filling degree In order to produce a layered structure with excellent high-temperature strength by the layered manufacturing method using metal powder, it is preferable to use a metal powder with a high filling degree, but in ordinary mechanical alloying, the desired sphericity is not obtained. Hard to get. In mechanical alloying, rolling and folding of particles, pressure contact and crushing of particles are repeated to form an alloy, so oxides are not necessarily dispersed on the surface.
  • the problem to be solved by the present invention is to provide a layered manufacturing powder having excellent high-temperature strength and a layered article manufactured using the layered manufacturing powder having excellent high-temperature strength.
  • oxide nanoparticles that have not been surface-treated with an organic substance are added to the surface of alloy particles that constitute the alloy powder.
  • ODS particle dispersion strengthening
  • an alloy powder material for additive manufacturing comprising an alloy powder and oxide nanoparticles attached to the surfaces of the alloy particles constituting the alloy powder and not subjected to a surface treatment with an organic substance.
  • the oxide constituting the oxide nanoparticles is any one of Y 2 O 3 , ThO 2 , Al 2 O 3 , TiO 2 and SiO 2 ]
  • the alloy powder material for additive manufacturing according to any one of [8] A metal laminate-molded article that has been laminate-molded using the alloy powder material for laminate manufacturing according to any one of [1] to [7].
  • oxide nanoparticle agglomerates tend to occur on the surfaces of the alloy particles that make up the alloy powder.
  • oxide nanoparticle aggregates diffuse in the melt pool during laser melting and are dispersed throughout, if the area ratio of the oxide nanoparticle aggregates becomes excessively large, oxide nanoparticle aggregation occurs. A part of the part is not completely dispersed and remains as a ⁇ m-scale oxide nanoparticle aggregation part. The remaining ⁇ m-scale oxide nanoparticle aggregates occur when the area ratio of the oxide nanoparticle aggregates exceeds 10%.
  • the oxide nanoparticle agglomeration part on the surface of the alloy particles constituting the alloy powder is suppressed to within 10%, when the alloy powder material for additive manufacturing is melted in the additive manufacturing method, the oxide nanoparticle agglomeration part will not be formed.
  • the agglomeration is dissolved, fine oxide nanoparticles of several tens to several hundred nm are dispersed, so that the layered product is strengthened by particle dispersion strengthening.
  • the area ratio of the oxide nanoparticle aggregation portion exceeds 10%, the aggregation of the oxide nanoparticle aggregation portion is not sufficiently dissolved during melting, and the ⁇ m-scale oxide nanoparticle aggregation portion tends to remain. This ⁇ m-scale oxide nanoparticle agglomerate may become a starting point of fracture and reduce the strength of the layered product.
  • the oxide nanoparticles By attaching the oxide nanoparticles to the surface of the alloy particles constituting the alloy powder, the oxide nanoparticles are positioned between the alloy particles.
  • the fluidity of the alloy powder material can be improved because the adhesive force acting between the particles of is reduced.
  • SEM scanning electron microscope
  • the alloy powder material for additive manufacturing of the present invention will be described below.
  • the alloy powder material for additive manufacturing of the present invention comprises alloy powder and oxide nanoparticles that are attached to the surface of the alloy particles that constitute the alloy powder and that are not surface-treated with an organic substance. Oxide nanoparticles adhere to the surfaces of at least some of the alloy particles constituting the alloy powder.
  • the alloy powder material for additive manufacturing of the present invention may contain alloy particles having no oxide nanoparticles attached to their surfaces. At least some of the oxide nanoparticles contained in the alloy powder material for additive manufacturing of the present invention adhere to the surface of the alloy particles.
  • the alloy powder material for additive manufacturing of the present invention may contain oxide nanoparticles that are not attached to the alloy particles.
  • Alloy powder is an aggregate of alloy particles.
  • the alloy powder is the base powder of the alloy powder material for additive manufacturing of the present invention.
  • the alloy powder is Ni-based alloy powder.
  • the Ni-based alloy powder may contain one or more elements selected from Fe, Cr, C, Mn, Si, Mo, Co, Nb, Al, Ti, Ta, Zr and B.
  • the content of each element is as follows.
  • the mass % is based on the mass of the alloy powder.
  • the Fe content is preferably 25.0% by mass or less, more preferably 20.0% by mass or less.
  • the lower limit of the Fe content may be 0% by mass or may be greater than 0% by mass.
  • the Cr content is preferably 28.0% by mass or less, more preferably 24.0% by mass or less.
  • the lower limit of the Cr content may be 0% by mass or may be more than 0% by mass.
  • the content of C is preferably 0.2% by mass or less, more preferably 0.1% by mass or less.
  • the lower limit of the C content may be 0% by mass or may be more than 0% by mass.
  • the content of Mn is preferably 0.2% by mass or less, more preferably 0.1% by mass or less.
  • the lower limit of the Mn content may be 0% by mass or may be more than 0% by mass.
  • the Si content is preferably 0.2% by mass or less, more preferably 0.1% by mass or less.
  • the lower limit of the Si content may be 0% by mass or may be more than 0% by mass.
  • the Mo content is preferably 4.0% by mass or less, more preferably 3.5% by mass or less.
  • the lower limit of the Mo content may be 0% by mass or may be more than 0% by mass.
  • the Co content is preferably 25.0% by mass or less, more preferably 21.0% by mass or less.
  • the lower limit of the Co content may be 0% by mass or may be more than 0% by mass.
  • the content of Nb is preferably 7.0% by mass or less, more preferably 6.0% by mass or less.
  • the lower limit of the Nb content may be 0% by mass or may be more than 0% by mass.
  • the Al content is preferably 6.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Al content may be 0% by mass or may be more than 0% by mass.
  • the content of Ti is preferably 6.0% by mass or less, more preferably 4.0% by mass or less.
  • the lower limit of the Ti content may be 0% by mass or may be more than 0% by mass.
  • the Ta content is preferably 4.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Ta content may be 0% by mass or may be more than 0% by mass.
  • the Zr content is preferably 1.0% by mass or less, more preferably 0.3% by mass or less.
  • the lower limit of the Zr content may be 0% by mass or may be more than 0% by mass.
  • the content of B is preferably 0.01% by mass or less, more preferably 0.005% by mass or less.
  • the lower limit of the B content may be 0% by mass or may be more than 0% by mass.
  • the balance of the Ni-based alloy powder consists of Ni and unavoidable impurities.
  • the alloy powder is Fe-based alloy powder.
  • the Fe-based alloy powder may contain one or more elements selected from Ni, Cr, C, Mn, Si, Nb, Cu, Mo, Ti and Al. The content of each element is as follows. In addition, the mass % is based on the mass of the alloy powder.
  • the Ni content is preferably 10.0% by mass or less, more preferably 5.0% by mass or less.
  • the lower limit of the Ni content may be 0% by mass or may be more than 0% by mass.
  • the Cr content is preferably 20.0% by mass or less, more preferably 18.0% by mass or less.
  • the lower limit of the Cr content may be 0% by mass or may be more than 0% by mass.
  • the content of C is preferably 0.3% by mass or less, more preferably 0.1% by mass or less.
  • the lower limit of the C content may be 0% by mass or may be more than 0% by mass.
  • the content of Mn is preferably 2.0% by mass or less, more preferably 1.0% by mass or less.
  • the lower limit of the Mn content may be 0% by mass or may be more than 0% by mass.
  • the Si content is preferably 2.0% by mass or less, more preferably 1.0% by mass or less.
  • the lower limit of the Si content may be 0% by mass or may be more than 0% by mass.
  • the content of Nb is preferably 5.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Nb content may be 0% by mass or may be more than 0% by mass.
  • the Cu content is preferably 7.0% by mass or less, more preferably 5.0% by mass or less.
  • the lower limit of the Cu content may be 0% by mass or may be more than 0% by mass.
  • the Mo content is preferably 5.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Mo content may be 0% by mass or may be more than 0% by mass.
  • the content of Ti is preferably 5.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Ti content may be 0% by mass or may be more than 0% by mass.
  • the Al content is preferably 5.0% by mass or less, more preferably 3.0% by mass or less.
  • the lower limit of the Al content may be 0% by mass or may be more than 0% by mass.
  • the balance of the Fe-based alloy powder consists of Fe and unavoidable impurities.
  • D 50 of the alloy powder is preferably 2 ⁇ m or more and 150 ⁇ m or less.
  • the D 50 of the alloy powder is less than 2 ⁇ m, excessive pulverization may significantly reduce the fluidity of the powder. If the D 50 of the alloy powder exceeds 150 ⁇ m, the powder filling rate may decrease and the density of the shaped body may decrease.
  • the preferred range of D 50 of the alloy powder varies depending on the additive manufacturing method. By adjusting the D 50 of the alloy powder according to the manufacturing method of the layered manufacturing, it is possible to appropriately obtain the layered product.
  • Preferred ranges of D 50 for alloy powders in laser powder sintering additive manufacturing (SLM), laser deposition, electron beam and binder jet are as follows. ⁇ Laser Powder Sintering Laminated Manufacturing (SLM): 10 ⁇ m ⁇ D 50 ⁇ 45 ⁇ m ⁇ Laser deposition method or electron beam method: 45 ⁇ m ⁇ D 50 ⁇ 150 ⁇ m ⁇ Binder jet method: 2 ⁇ m ⁇ D 50 ⁇ 25 ⁇ m
  • the D 50 ( ⁇ m) of the alloy powder is the particle diameter at the point where the cumulative volume is 50% in the volume-based cumulative frequency distribution curve obtained when the total volume of the alloy powder is 100%.
  • D50 is measured by the laser diffraction scattering method.
  • a laser diffraction/scattering particle size distribution measuring apparatus "Microtrac MT3000" manufactured by Nikkiso Co., Ltd. is used as an apparatus suitable for this measurement. Powder is poured into the cell of this device together with pure water, and the particle size is detected based on the light scattering information of the particles.
  • Examples of methods for producing alloy powder include water atomization, single roll quenching, twin roll quenching, gas atomization, disc atomization, and centrifugal atomization.
  • the single roll cooling method, the gas atomization method and the disc atomization method are preferable for producing the alloy powder.
  • powder can be obtained by pulverizing by mechanical milling or the like.
  • the milling method include a ball mill method, a bead mill method, a planetary ball mill method, an attritor method, a vibration ball mill method, and the like.
  • the gas atomization method is particularly preferred as the method for producing the alloy powder.
  • the primary particle size of the oxide nanoparticles is preferably 1 nm or more and 100 nm or less.
  • the primary particle size of the oxide nanoparticles after mixing the alloy powder and the oxide nanoparticles (after attaching the oxide nanoparticles to the alloy particles constituting the alloy powder) is the same as that of the oxide nanoparticles before mixing. It is the same as the primary particle size of the particles, and the primary particle size of the oxide nanoparticles can be determined based on the specific surface area measurement (JIS Z 8830:2013) by the gas adsorption method.
  • the average primary particle size of the oxide nanoparticles is preferably 10 nm or more and 100 nm or less.
  • the average primary particle size of oxide nanoparticles can be obtained based on specific surface area measurement (JIS Z 8830: 2013) by a gas adsorption method.
  • the amount of oxide nanoparticles added to the alloy powder is, for example, 0.02% by mass or more and 1.75% by mass, preferably 0.1% by mass or more and 1.5% by mass or less, based on the mass of the alloy powder. . If the amount of oxide nanoparticles added is less than 0.1% by mass, the effect of particle dispersion strengthening (ODS) may not be sufficiently obtained. If the amount of oxide nanoparticles added exceeds 1.5% by mass, oxide nanoparticle aggregates are likely to occur, and the strength of the layered product may decrease.
  • the amount of oxide nanoparticles added is more preferably 0.2% by mass or more and 1.5% by mass or less, and still more preferably 0.25% by mass or more and 1.0% by mass or less, based on the mass of the alloy powder. be.
  • the amount of oxide nanoparticles added is sufficient to be 0.01% by mass or more and less than 0.1% by mass based on the mass of the alloy powder, but particle dispersion strengthening (ODS) In order to achieve this, it is preferable to add 0.1% by mass or more of oxide nanoparticles. When the amount of oxide nanoparticles added is increased to 0.1% by mass or more, oxide nanoparticle aggregates of 1 ⁇ m or more are inevitably generated.
  • Examples of methods for producing oxide nanoparticles that have not been surface-treated with an organic substance include a flame spray pyrolysis method (FSP method) and a physical vapor synthesis method. be done.
  • FSP method flame spray pyrolysis method
  • a physical vapor synthesis method be done.
  • FSP method flame spray pyrolysis method
  • it is effective to use oxide nanoparticles with a high degree of sphericity.
  • the sphericity is higher than that of the oxide nanoparticles obtained by the FSP method, and it is easier to obtain a preferable powder.
  • oxides constituting oxide nanoparticles include Y 2 O 3 , ThO 2 , Al 2 O 3 , TiO 2 and SiO 2 .
  • the oxide nanoparticles may be composed of one kind of oxide, or may be composed of two or more kinds of oxides. Any oxide nanoparticles that can stably exist in a matrix even at high temperatures can be suitably used without being limited to these oxides. Of these, Y 2 O 3 and Al 2 O 3 are preferred because they can stably exist in the matrix even at high temperatures. Y 2 O 3 is more preferred. In the examples, Y 2 O 3 is used as a representative oxide nanoparticle.
  • Oxide nanoparticles are not surface-treated with organic substances.
  • surface treatment with organic substances include surface treatment with organic substances such as dimethylsilyl and trimethylsilyl.
  • the area ratio of the oxide nanoparticle aggregates formed by the oxide nanoparticles adhering to the surface of the alloy particles is, for example, 13% or less, preferably 10% or less.
  • the area ratio of the oxide nanoparticle agglomeration part is 10% or less
  • the alloy powder material for additive manufacturing is melted in the additive manufacturing method, the aggregation of the oxide nanoparticles is dissolved and the size of several tens of ⁇ m to several hundred ⁇ m is reduced. Because it is dispersed as fine oxide nanoparticles, the laminate is reinforced with ODS.
  • the area ratio of the oxide nanoparticle aggregated portions exceeds 10%, the oxide nanoparticles are not sufficiently deaggregated during melting, and ⁇ m-scale oxide nanoparticle aggregated portions remain. Since the ⁇ m-scale oxide nanoparticle agglomeration part can be a starting point of destruction, there is a possibility that the strength of the laminate-molded body is lowered.
  • the area ratio of the oxide nanoparticle aggregates is more preferably 7% or less, and even more preferably 5% or less.
  • the area ratio of the oxide nanoparticle aggregation part is preferably 0.1% or more, more preferably 0.5% or more, and even more preferably 0.9% or more. be. Each of these lower limits may be combined with any of the above upper limits. In a preferred embodiment, the area ratio of the oxide nanoparticle aggregates is 0.1% or more and 10% or less.
  • the area ratio of the oxide nanoparticle aggregation part is obtained from the above formula, and the average value thereof is used as the oxide nanoparticle in the alloy powder material for additive manufacturing of the present invention. It is defined as the area ratio of the particle aggregation portion.
  • the alloy powder material for additive manufacturing of the present invention can be produced by mixing alloy powder and oxide nanoparticles. Mixing can be done using a V-blender. Mixing can also be done with a tumbler mixer, ball mixer, or other mechanical device. It is also possible to put them in a container and mix them manually.
  • oxide nanoparticles that do not adhere to the particles that make up the alloy powder may remain.
  • the remaining oxide nanoparticles have a size of several ⁇ m to several hundred ⁇ m.
  • These unattached oxide nanoparticles are preferably removed by sieve classification. Through this removal step, a more suitable alloy powder material for additive manufacturing can be obtained.
  • the metal laminate modeled article of the present invention will be described below.
  • the metal laminate-molded article of the present invention is a metal laminate-molded article that has been laminate-molded using the alloy powder material for laminate manufacturing of the present invention.
  • Typical methods of the additive manufacturing method include, for example, the laser powder sintering additive manufacturing (SLM) method, the binder jet method, the electron beam powder sintering additive manufacturing (EBM) method, and the laser deposition method.
  • SLM laser powder sintering additive manufacturing
  • EBM electron beam powder sintering additive manufacturing
  • the laminate manufacturing method can be performed using, for example, a 3D printer.
  • the material used in the additive manufacturing method is preferably composed only of the alloy powder material for additive manufacturing of the present invention. agent).
  • alloy powders having the component compositions shown in Table 1-1 were produced by the gas atomization method.
  • the gas atomization method raw materials mixed to a predetermined distribution in an alumina crucible are melted by high-frequency induction heating in a vacuum, and the molten alloy is dropped from a nozzle with a diameter of about 5 mm under the crucible, and high pressure argon or It was carried out by gas atomization with high pressure nitrogen.
  • Ni-based alloy powder corresponding to Inconel 718 (No. A) Fe-52% Ni-20% Cr-0.05% C-0.1% Mn-0.2% Si-3.0% Mo-0.3% Co-5.2% Nb - 0.5% Al - 0.9% Ti - 0.003% B, (No.
  • Table 1-2 shows the average particle size D 50 ( ⁇ m) and sphericity of the obtained alloy powder.
  • the average particle diameter D 50 is the particle diameter at the point where the cumulative volume is 50% in the volume-based cumulative frequency distribution curve obtained when the total volume of the alloy powder is 100%.
  • the method for measuring D50 is as follows.
  • S is the projected area of the particle or its cross section
  • L is the contour length of this projected image.
  • an image analyzer (Morphologi G3) is used.
  • Method for measuring D50 In the measurement of the average particle diameter D50 , the total volume of the alloy powder is assumed to be 100%, and the cumulative curve is obtained. The particle diameter at the point on this curve where the cumulative volume is 50% is D50 . Particle diameter D 50 is measured by laser diffraction scattering method. As an apparatus suitable for this measurement, Nikkiso's laser diffraction/scattering particle size distribution measuring apparatus "Microtrac MT3000" can be mentioned. Powder is poured into the cell of this device together with pure water, and the particle size is detected based on the light scattering information of the particles.
  • the oxide nanoparticles may remain without adhering to the alloy particles constituting the alloy powder.
  • the remaining oxide nanoparticles have a size of several ⁇ m to several hundred ⁇ m. Therefore, unattached oxide nanoparticles were removed by sieve classification. Through this removal step, a more suitable alloy powder material for additive manufacturing can be obtained.
  • the "area of one alloy particle" was measured only for the portion visible in the SEM image (that is, the portion that overlapped and was not visible was not measured).
  • the area ratio of the oxide nanoparticle aggregation part is obtained from the above formula, and the average value thereof is used as the oxide nanoparticle aggregation part in the alloy powder material for additive manufacturing. area ratio.
  • the Hausner ratio of the alloy powder material for additive manufacturing is an index defined by tap density/apparent density. The lower the Hausner ratio, the better the fluidity of the powder.
  • the tap density (g/cm 3 ) was evaluated by filling about 50 g of powder into a cylinder with a volume of 100 cm 3 , dropping height of 10 mm, and tapping 200 times. The apparent density (g/cm 3 ) was measured according to JIS Z 2504:2012.
  • the Ni-based alloy powder A, Ni-based alloy powder B, or Fe-based alloy powder C shown in Table 1-1 was oxidized while changing the amount of oxide nanoparticles added.
  • Example no. 1 to 11 alloy powder materials for additive manufacturing and comparative example No. Nos. 12 to 14 alloy powder materials for additive manufacturing were produced, additively manufactured, and their properties were evaluated by the above-described method.
  • the results are shown in Tables 2 and 3.
  • All of the oxide nanoparticles used in Examples and Comparative Examples are Y 2 O 3 nanoparticles.
  • the amount of oxide nanoparticles added is based on the mass of the alloy powder, which is the base powder.
  • All of the laminate-molded bodies produced using the alloy powder material for additive manufacturing of the examples whose base powder is the Ni-based alloy powder A are the alloy powder materials for additive manufacturing of the comparative example whose base powder is the Ni-based alloy powder A.
  • the laminate-molded body produced using the alloy powder material for additive manufacturing of the example whose base powder is the Ni-based alloy powder B is obtained by using the alloy powder material for additive manufacturing of the comparative example whose base powder is the Ni-based alloy powder B.
  • the tensile strength was high and it was difficult to break, and it exhibited excellent high-temperature strength.
  • All of the laminate-molded bodies produced using the alloy powder material for additive manufacturing of the examples whose base powder is the Fe-based alloy powder C are the alloy powder materials for additive manufacturing of the comparative example whose base powder is the Fe-based alloy powder C. Compared to the laminate-molded body produced using the alloy powder material for additive manufacturing of the examples whose base powder is the Fe-based alloy powder C.
  • alloy powder materials for additive manufacturing of Examples had a low Hausner ratio and exhibited excellent fluidity, and were suitable as alloy powder materials for additive manufacturing.
  • Comparative example No. 13 and No. No. 14 had poor fluidity and did not flow, so the apparent density could not be measured and the Hausner ratio could not be evaluated.
  • conventional alloy powder materials are not suitable for additive manufacturing, by adding oxide nanoparticles as in the present invention, applications for additive manufacturing are secured, and high-temperature strength is also excellent. became a thing.
  • the alloy powder material for additive manufacturing of the present invention is suitable for metal powder for additive manufacturing using the metal deposition method, the powder bed method, the electron beam method, and the binder jet method.
  • laminate-molded bodies are suitable for heat-resistant parts.

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