WO2020250811A1 - 積層造形用銅粉末、積層造形体、積層造形体の製造方法および積層造形装置 - Google Patents

積層造形用銅粉末、積層造形体、積層造形体の製造方法および積層造形装置 Download PDF

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WO2020250811A1
WO2020250811A1 PCT/JP2020/022203 JP2020022203W WO2020250811A1 WO 2020250811 A1 WO2020250811 A1 WO 2020250811A1 JP 2020022203 W JP2020022203 W JP 2020022203W WO 2020250811 A1 WO2020250811 A1 WO 2020250811A1
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Prior art keywords
laminated
powder
copper powder
copper
less
Prior art date
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Ceased
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PCT/JP2020/022203
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English (en)
French (fr)
Japanese (ja)
Inventor
雄史 杉谷
秀樹 京極
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Fukuda Metal Foil and Powder Co Ltd
Technology Research Association for Future Additive Manufacturing (TRAFAM)
Original Assignee
Fukuda Metal Foil and Powder Co Ltd
Technology Research Association for Future Additive Manufacturing (TRAFAM)
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Application filed by Fukuda Metal Foil and Powder Co Ltd, Technology Research Association for Future Additive Manufacturing (TRAFAM) filed Critical Fukuda Metal Foil and Powder Co Ltd
Priority to JP2021526057A priority Critical patent/JP7544697B2/ja
Priority to US17/607,736 priority patent/US12358076B2/en
Priority to EP20822132.5A priority patent/EP3950176A4/en
Priority to CN202080040371.6A priority patent/CN113939605B/zh
Publication of WO2020250811A1 publication Critical patent/WO2020250811A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/34—Laser welding for purposes other than joining
    • B23K26/342—Build-up welding
    • 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
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F1/12—Metallic powder containing non-metallic 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
    • B22F10/20—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
    • 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
    • B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B22F12/90—Means for process control, e.g. cameras or sensors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/03—Press-moulding apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • 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
    • B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories therefor
    • 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
    • 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
    • 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
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • 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
    • C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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
    • B22F2301/10—Copper
    • 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
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/08—Non-ferrous metals or alloys
    • B23K2103/12—Copper or alloys thereof
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present invention relates to laminated modeling with copper powder.
  • Patent Document 1 a layer of nanosilica (SiO 2 ) of less than 100 ppm is formed as a treatment agent on the surface of Inconel 718 (registered trademark: Inconel 718), which is a nickel alloy, in an additional manufacturing technique (3D printing technique).
  • 3D printing technique A technique for improving the flow and diffusion characteristics of a metal powder is disclosed.
  • Patent Document 2 describes a metal powder having an average diameter of 10 ⁇ m or more and 200 ⁇ m or less made of an alloy such as Al, Co, Cr, Fe, and Ni, and a metal powder having a higher sphericity and an average diameter than the metal powder.
  • a mixture with a powder of ceramic, silica or alumina having a body integral ratio of 0.001% or more and 1% or less of the metal powder, which is 1/10 or less of the body, as a powder for laminated molding fluidity is obtained.
  • the technology for improving the above is disclosed.
  • An object of the present invention is to provide a technique for solving the above-mentioned problems.
  • the copper powder for laminated molding according to the present invention is used. It is a copper powder for laminated modeling in which nanooxide of 0.01 wt% or more and 0.20 wt% or less is mixed with copper powder.
  • the laminated model according to the present invention A laminated model formed by using the copper powder for laminated modeling. It contains 0.01 wt% or more and 0.20 wt% or less of nanooxide, and has an electric conductivity of 80% IACS or more.
  • the method for manufacturing a laminated model according to the present invention is: It is a manufacturing method of a laminated model which manufactures a laminated model using the copper powder for laminated model.
  • the layered manufacturing copper powder was spread in layers, by irradiating while scanning a laser beam so that the energy density is 500 J / mm 3 or more 1500 J / mm 3 or less laser output 1kW less, laminated one layer
  • the laminated modeling apparatus In order to achieve the above object, the laminated modeling apparatus according to the present invention
  • the average particle size of the copper powder is 5 ⁇ m or more and 15 ⁇ m or less
  • the powder resistance value of the copper powder for laminated molding containing the copper powder is (7.50E + 5) ⁇ or more and (2.50E + 7) ⁇ or less.
  • Judgment unit to judge that When both the judgment results by the judgment unit are within the range, the laminated modeling unit that models the laminated modeling body using the copper powder for laminated modeling and the laminated modeling unit. To be equipped.
  • FIG. 5 shows a scanning electron microscope (SEM) image of the surface of a laminated model of pure copper produced from a mixed powder of pure copper powder having an average particle diameter of 9.6 ⁇ m and 0.10 wt% nanooxide in an example of the present invention. is there.
  • FIG. 5 shows a scanning electron microscope (SEM) image of the surface of a laminated model of pure copper produced from a mixed powder of pure copper powder having an average particle diameter of 9.6 ⁇ m and 0.10 wt% nanooxide in an example of the present invention. is there.
  • FIG. 5 shows a scanning electron microscope (SEM) image of the surface of a laminated model of pure copper produced from a mixed powder of pure copper powder having an average particle diameter of 13.5 ⁇ m and 0.01 wt% nanooxide in an example of the present invention. is there.
  • SEM scanning electron microscope
  • the pure copper powder used in the present embodiment is fine in the fields of electric circuit connectors, heat sinks, heat exchangers, etc., if a laminated model using pure copper powder, which is used as a material for laminated modeling, can be produced. It is possible to make various shapes.
  • the laminated model using pure copper powder has a sufficient density (measured density by Archimedes method is 98.5% or more). If the measurement density is less than 98.5%, problems such as water leakage will occur. Further, when utilizing the electrical conductivity and thermal conductivity of copper, it is desirable to have sufficient electrical conductivity (80% IACS or more) as a pure copper product.
  • the laminated model using pure copper powder is not limited to the above example, and may be used as a circuit component or an electromagnetic wave shield component.
  • ⁇ Copper powder for laminated modeling Generally, in metal laminated molding, a fiber laser is used as a heat source in laser beam laminated molding, and an arbitrary shape is formed by melting and solidifying metal powder. In this case, a material having a low electric conductivity can obtain a high-density model, but a material having a high electric conductivity often cannot obtain a high-density model. Copper is an element with high electrical conductivity and thermal conductivity, and it is expected to produce electrically conductive parts and heat conductive parts with complicated shapes using laser beam laminated molding, but pure copper powder produces a high-density model. Cannot be made. The reason is that when pure copper powder is used, the thermal energy is diffused during laser irradiation due to its high electrical conductivity, and the laser beam is reflected during laser irradiation, so the thermal energy required for the pure copper powder to melt. This is because
  • the electric conductivity is reduced and the density is sufficient (measured density by the Archimedes method is 98.5% or more). It has become possible to manufacture a laminated model.
  • the electric conductivity of the laminated model is about 50% IACS, and the electric conductivity of the laminated model is 80% IACS. It cannot be more than that.
  • the electric conductivity is lower than that of pure copper powder, and it is possible to melt with an existing device having an energy density of about 1000 J / mm 3 , and the pure copper laminated model has high density and high conductivity.
  • a copper powder for laminated molding which can be obtained.
  • the electrical conductivity of the copper powder for laminated molding is lower than that of pure copper powder.
  • the powder resistance value is twice or more that of pure copper powder.
  • the powder resistance value of the copper powder for laminated molding containing copper powder is in the range of (7.50E + 5) ⁇ to (2.50E + 7) ⁇ .
  • a powder bed can be formed from copper powder for laminated modeling.
  • the fluidity (JIS Z2502 / FR: flow rate) of the copper powder for laminated molding is in the range of 15 to 120 sec / 50 g, preferably 60 sec / 50 g or less.
  • the adhesive force (FT4 measurement) of the copper powder for laminated modeling is 0.450 kPa or less. By satisfying this condition, it can be used as a metal powder for laminated modeling in the powder bed method.
  • the content of pure copper powder in the copper powder for laminated modeling is at least specified.
  • the apparent density (JIS Z2504) of copper powder for laminated modeling shall be in the range of 4.0 to 5.5 g / cm 3 .
  • the amount of copper per unit volume of the powder bed is kept constant, and the laminated model can have the characteristics of pure copper.
  • FIG. 1 is a diagram showing a schematic configuration example of the laminated modeling apparatus 10 of the present embodiment.
  • the laminated modeling unit of the laminated modeling device 10 includes an electron beam or fiber laser 11a emission mechanism 11, a hopper 12 which is a powder tank, and a squeezing blade 13 for forming a powder bed in which powder is spread in layers with a constant thickness. And a table 14 that repeats lowering by a certain thickness for lamination. The collaboration between the squeezing blade 13 and the table 14 produces a uniform and constant thickness powder additive 15.
  • each layer is irradiated with a fiber laser 11a based on slice data obtained from 3D-CAD data, and a metal powder (copper powder in this embodiment) is melted to produce a laminated model 15a.
  • the laminated modeling powder determination unit 16 determines whether or not the laminated modeling powder can be laminated and modeled by the laminated modeling device 10.
  • the average particle size of the copper powder is in the range of 5 ⁇ m to 15 ⁇ m
  • the powder resistance value of the copper powder for laminated molding containing the copper powder is from (7.50E + 5) ⁇ . Judge that it is within the range of (2.50E + 7) ⁇ .
  • a pure copper laminated model having a relative density of 99% or more and an electric conductivity of 80% IACS or more can be produced with the energy density possible in the laminated modeling device 10.
  • t the thickness of the powder bed
  • P the laser output
  • v the scanning speed of the laser
  • s the laser scanning pitch.
  • the laminated model using pure copper powder has a sufficient density.
  • the measured density by the Archimedes method is 98.5% or more.
  • the laminated model using pure copper powder has sufficient electrical conductivity as a pure copper product.
  • the electrical conductivity is 80% IACS or higher. By satisfying this condition, it can be used as a laminated model having the characteristics of pure copper.
  • Copper powder for laminated modeling of this embodiment is a laminated molding copper powder that satisfies the above conditions, can be melted by an existing device having a laser output of 1 kW or less and an energy density of about 1000 J / mm 3 , and can form a powder bed.
  • the following powders are provided as copper powders for laminated molding having a desired strength as a pure copper laminated molded product after molding and having sufficient electric conductivity.
  • nanooxide those having a shape close to a sphere or a true sphere and having a primary average particle diameter in the range of 10 nm to 100 nm, particularly 50 nm or less are preferably used.
  • Such nano-oxide for example, outside of nanosilica (SiO 2), as shown in Table 1 below, nano copper oxide (CuO), nano alumina (Al 2 O 3), nanotitania (TiO 2), nano Yttria (Y 2 O 3 ) and the like are included.
  • the average particle size of pure copper powder shall be in the range of 5 ⁇ m to 15 ⁇ m. That is, in the present embodiment, the amount of energy required for one particle to melt is reduced by reducing the volume of one particle of pure copper metal particles, and an existing device having an energy density of about 1000 J / mm 3 is used. For example, pure copper powder having an average particle size of 20 ⁇ m or less is used so that it can be melted.
  • the average particle size of the pure copper powder is less than 5 ⁇ m, sufficient fluidity cannot be obtained even if nanooxides are mixed, and the formation of a powder bed that realizes laminated molding is poor. Further, if the particles are made too small, the amount of metal existing in the powder bed decreases (corresponding to a decrease in apparent density), so that modeling cannot be performed due to poor formation of the powder bed. Therefore, a pure copper model with high density and high conductivity cannot be obtained. On the other hand, when the average particle size of the pure copper powder is 15 ⁇ m or more, a pure copper model having high density and high conductivity cannot be obtained even if a powder bed can be formed. It is more desirable that the average particle size of the pure copper powder is in the range of 8 ⁇ m to 15 ⁇ m.
  • FIG. 2 is a schematic view illustrating a mixed state of pure copper powder and nanooxide in the copper powder for laminated molding in the present embodiment.
  • the dimensions of the pure copper powder and the nanooxide are different from the actual ones, and the nanooxide is so small that it cannot be shown.
  • the pure copper powder 21 has high electrical conductivity and high thermal conductivity because each of the pure copper particles 20 is in direct contact with each other, and as shown by the arrow 22, the heat of the portion irradiated with the laser beam is the adjacent pure copper particles. It conducts heat through 20 and diffuses. Therefore, in an existing device having an energy density of about 1000 J / mm 3 , heat cannot be accumulated and melted before the portion irradiated with the laser beam exceeds the melting point.
  • the nanooxide 26 is interrupted between the pure copper particles 20, and the electric conductivity and the thermal conductivity between the pure copper particles 20 are reduced.
  • the heat generated by the laser beam is accumulated in each of the pure copper particles 20. Therefore, in an existing device having an energy density of about 1000 J / mm 3 , heat can be accumulated and melted before the portion irradiated with the laser beam exceeds the melting point.
  • Non-Patent Document 1 It is known as the Wiedemann-Franz law in Non-Patent Document 1 and the like that the reduction in electrical conductivity is proportional to the reduction in thermal conductivity in the copper powder for laminated molding of pure copper powder in the present embodiment. ..
  • the 50% particle size ( ⁇ m) of the copper powder for laminated molding was measured by a laser diffraction method (Microtrack MT3300: manufactured by Microtrack Bell Co., Ltd.).
  • FIG. 6A is a diagram showing a configuration of a shear stress measuring unit 60 for measuring a shear stress in the present embodiment.
  • the shear stress measuring unit 60 measures the shear stress by the rotary cell method, places the rotary cell 61 having a blade with a blade attached to the lower part inside the outer cell 62, and puts the powder to be measured on the upper part of the outer cell 62. Fill. Shear stress is measured from the rotational torque of the rotating cell 61 while applying a predetermined normal stress from the rotating cell 61 toward the outer cell 62.
  • FIG. 6B is a diagram showing a method of obtaining an adhesive force based on the shear stress measured by the shear stress measuring unit 60 in the present embodiment.
  • a plot of shear stress measured when shear occurs under each normal stress by the shear stress measuring unit 60 is called a fracture envelope, and powder is applied by applying a stronger shear stress than the fracture envelope. Shearing occurs in the body layer.
  • the shear stress when the normal stress is 0 (zero) on the fracture envelope (for example, 65) is obtained as the adhesive force between the particles.
  • the apparent density (g / cm 3 ) of the copper powder for laminated molding was measured according to JIS Z2504.
  • the fluidity (sec / 50 g) of the copper powder for laminated molding was measured according to JIS Z2502.
  • FIG. 3B is a diagram showing a method for measuring the powder resistance value of the mixed powder of pure copper powder and nanooxide according to the present embodiment.
  • the powder resistance measuring instrument 39 is an insulator having two copper plates 32 for measuring terminals connected to both terminals of the resistance measuring instrument 35 by cables 36 and 37 having contact terminals, and a hole for accommodating the powder to be measured 31. 33 and two upper and lower insulators 34 for pressing for strongly connecting the two copper plates 32 for measurement terminals to the powder to be measured 31 are provided.
  • the insulators 33 and 34 are made of elastic rubber or the like.
  • the holes for accommodating the powder to be measured 31 have a thickness of 0.3 mm (corresponding to the thickness of the insulator 33) and a diameter of 17 mm, but are not limited.
  • the powder to be measured 31 may be filled without voids and may have sufficient electrical connection with the two copper plates 32 for measurement terminals.
  • FIG. 3C is a diagram showing a method for measuring the powder resistance value of the mixed powder of pure copper powder and nanooxide according to the present embodiment.
  • the same components as those in FIG. 3B are designated by the same reference numbers, and duplicate description will be omitted.
  • FIG. 7 is a diagram showing a test example of whether or not a powder bed can be formed by skiing the copper powder for laminated modeling with the laminated modeling device 10 in the present embodiment.
  • FIG. 7 shows a powder bed in a formable state 71 and a non-formable state 72.
  • the electrical conductivity (% IACS) of the pure copper laminated model was measured with an eddy current type conductivity meter.
  • the density (%) of the pure copper laminated model was measured based on the ratio obtained by dividing the void area by the area of the cross-sectional SEM image.
  • FIG. 3A is a diagram showing changes in the powder resistance value 30 of the mixed powder of pure copper powder and nanooxide according to the present embodiment.
  • the powder resistance value was measured by the powder resistance measuring device 39 shown in FIGS. 3B and 3C.
  • the powder resistance value 30 was increased by a value larger than 10 times in pure copper powder having an average particle size of 20 ⁇ m or less by adding and mixing nanooxides.
  • FIG. 4 is a diagram showing the thermal energy required for melting the pure copper powder of the present embodiment.
  • the upper 41 of FIG. 4 shows the energy density at which the density of the modeled object in each copper powder is 99% or more.
  • the lower 42 of FIG. 4 shows the energy density required for the pure copper powder predicted from the copper alloy powder containing tin (Sn) and the copper alloy powder containing phosphorus (P), and the copper powder for laminated molding of the present embodiment. It is a graph which contrasts with energy density.
  • the black triangles represent the electrical conductivity of the copper alloy powder containing tin (Sn) and the copper alloy powder containing phosphorus (P), and the relative density of the model formed by melting by laser irradiation of 99% or more. It is a plot of the relationship with the thermal energy required to become.
  • the straight line 43 connecting these black triangles shows the correspondence between the electric conductivity and the thermal energy required for melting by laser irradiation.
  • the thermal energy 44 is expected to be 5000 J / mm 3 or more as shown by the white ⁇ .
  • the density is high and the conductivity is high within the range where melting is possible with an existing device having an energy density of about 1000 J / mm 3. It is possible to provide a copper powder for laminated molding that can obtain a pure copper molded body of.
  • FIG. 5 is a diagram showing the energy density in the case of producing a laminated model from the mixed powder of pure copper powder and nanooxide according to the present embodiment and the electric conductivity of the produced laminated model of pure copper. ..
  • the upper 51 of FIG. 5 shows Comparative Examples 211 to 212 having an average particle size of 28.6 ⁇ m without adding and mixing nanooxides, which produced a copper laminated model in this example, and an average particle size of 19.9 ⁇ m with and without adding nanooxides.
  • the lower 52 of FIG. 5 is a graph plotted on the horizontal axis (energy density) / vertical axis (electrical conductivity) according to the value of the upper 51. From the lower 52 of FIG. 5, but not the electric conductivity of 80% IACS or less in only the molding near the energy density 1000 J / mm 3 in the comparative example (see 54), shaped in the vicinity of the energy density of 1000 J / mm 3 in the embodiment Then, a pure copper laminated model having an electric conductivity of 80% IACS or more can be obtained (see 53).
  • Suitable composition of copper powder for laminated molding by adding nanooxide to the pure copper powder, the conditions of the above-mentioned copper powder for laminated molding are satisfied, and the laminated molded body after the laminated molding by the laminated molding apparatus has the above-mentioned sufficient density and pure copper.
  • a pure copper powder having a sufficiently high electric conductivity as a product.
  • 0.01 wt% to 0.20 wt% (100 ppm to 2000 ppm) of nanooxide is mixed with the copper powder.
  • the average particle size of the copper powder is in the range of 5 ⁇ m to 15 ⁇ m.
  • 0.01 wt% to 0.10 wt% (100 ppm to 1000 ppm) of nanooxides are mixed in the average particle size of the copper powder in the range of 8 ⁇ m to 15 ⁇ m.
  • the nanooxide contains SiO 2
  • the primary average particle size of the nanooxide is in the range of 10 nm to 100 nm.
  • the powder resistance value of the copper powder for laminated molding is 10 to 100 times the powder resistance value of the copper powder, and is within the range of (7.50E + 5) ⁇ to (2.50E + 7) ⁇ . is there.
  • the bulk electrical conductivity of the copper powder is 100% JACS or higher.
  • the fluidity of the copper powder for laminated molding measured by JIS Z2502 is from 15 sec / 50 g to 120 sec / 50 g.
  • the volume is set so that one particle can be melted by a fiber laser, and by blending nanooxide, the fluidity of the powder is improved, and the metal in the powder bed
  • the apparent density which is an index of the amount, to 4.0 to 5.5 g / cm 3
  • the amount of copper per unit volume of the powder bed becomes constant.
  • connection between particles is hindered, the contact point between particles is reduced, the resistance value of powder is increased, and pure copper that is difficult to melt due to its high electrical conductivity is produced. Make it easier to melt.
  • the electrical conductivity of the modeled object when modeled under the condition that the energy density that can be calculated from the laser power, scan speed, scan pitch, and powder stack thickness is 1333 to 533 J / mm 3 is the eddy current ET using sigma check. It is possible to form a laminated model with 80% IACS or more by the measurement method.
  • the powder bed cannot be formed by the laminated molding apparatus 10 in the pure copper powder 300 to 600 having an average particle diameter of 20 ⁇ m or less.
  • the powder bed can be formed by the laminated modeling device 10, but from Tables 3 and 4 described later, the laminated model is formed by the laminated modeling device 10. Even so, the electrical conductivity is in the 60% IACS range, and a pure copper model that exceeds 80% IACS cannot be obtained.
  • nanooxides were added and mixed with pure copper powders 300 to 600 having an average particle diameter of 20 ⁇ m or less for which a powder bed could not be formed by the laminated molding apparatus 10.
  • FIG. 9A shows product information of AEROSIL® RX 300.
  • the upper 91 is product information
  • the lower 92 is a relational graph for converting "specific surface area" into particle diameter.
  • the specific surface area is 180-220 m 2 / g, so the particle size is on the order of 10 nm.
  • FIG. 9B shows an SEM image of AEROSIL® RX 300 (SEM ⁇ 1000).
  • a pure copper laminated model was produced by the laminated modeling apparatus 10 by selecting from the copper powders for laminated modeling that can form a powder bed in Tables 2 and 3.
  • the energy density was changed.
  • the energy density is related, for example, to Laser Power, Scanning Speed, Scanning Pitch, and Powder Layer.
  • the pure copper laminated model shown in Examples 411 to 413 and 513 to 534 achieves the electrical conductivity of the model at 80% IACS or more, which is the target in the present embodiment. Further, as shown in Table 41 of FIG. 4, the relative density of the modeled body also exceeds 99%.
  • FIG. 10A to 10D show SEM images ( ⁇ 50) of the surfaces of the laminated model in Examples and Comparative Examples.
  • FIG. 10A is an SEM image ( ⁇ 50) of the surface of a laminated model of pure copper of Example 531 (an example in which 0.10 wt% nanooxide was added and mixed with pure copper particles having an average particle diameter of 9.6 ⁇ m).
  • FIG. 10B is an SEM image ( ⁇ 50) of the surface of a laminated model of pure copper of Example 412 (an example in which 0.01 wt% nanooxide is added and mixed with pure copper particles having an average particle diameter of 13.5 ⁇ m).
  • FIG. 10A is an SEM image ( ⁇ 50) of the surface of a laminated model of pure copper of Example 531 (an example in which 0.10 wt% nanooxide was added and mixed with pure copper particles having an average particle diameter of 9.6 ⁇ m).
  • FIG. 10B is an SEM image ( ⁇ 50) of the surface of a laminated model of pure copper of Example
  • FIG. 10C is an SEM image ( ⁇ 50) of the surface of a laminated model of pure copper of Comparative Example 312 (an example in which 0.01 wt% nanooxide is added and mixed with pure copper particles having an average particle diameter of 19.9 ⁇ m).
  • FIG. 10D is an SEM image ( ⁇ 50) of Comparative Example 212 (the surface of a laminated model of pure copper of pure copper particles having an average particle diameter of 28.6 ⁇ m).
  • the surface of the laminated model is dense and has few irregularities, so that the relative density and the electric conductivity are high.
  • the surface of the laminated model has voids and irregularities. It is unlikely that the relative density and electrical conductivity will increase because of this.
  • the particle size becomes smaller depending on the surface condition, so that the laser melts stably and the surface becomes smooth.
  • the particle size becomes large, the melting of the laser becomes unstable and the molten copper becomes spheroidized, resulting in an uneven molding surface. It can be seen that due to this unevenness, holes are generated in the modeled body, causing a decrease in the modeling density.
  • the pure copper laminated model produced by using the powder for laminated modeling of the example has (conditions as a pure copper laminated model) "relative density of 99% or more" and “electrical conductivity of 80% IACS or more”. Has been achieved, and the conditions for a pure copper laminated model are satisfied.
  • the powder to which the nanooxide of this example was added and mixed it was compared with the characteristics of the pure copper laminated model produced by the laminated modeling apparatus 10.
  • a laminated model having a relative density of 99% or more is produced by an existing apparatus having an energy density of about 1000 J / mm 3. It was possible to provide a pure copper laminated model having an electric conductivity of 80% IACS or more as expected from the bulk electric conductivity.
  • Table 7 shows the results of each characteristic measurement shown in ⁇ Measurement of characteristics of copper powder for laminated molding >> for a copper powder material to which nanooxides other than SiO 2 shown in Table 1 were added and mixed. Shown.
  • the fluidity should not hinder the formation of the powder bed, and the powder resistance should be (1.00E + 4) ⁇ or more.
  • the powder resistance should be (1.00E + 4) ⁇ or more.
  • a copper laminated model having an electric conductivity of 60% IACS or more can be produced.
  • the powder resistance is in the range of (7.50E + 5) ⁇ or more and (2.50E + 7) ⁇ or less, the electric conductivity can achieve 80% IACS or more. Comparing with the test results of the copper powder material to which SiO 2 is added and mixed, the following points can be seen from the results of the powder characteristics in Table 7.
  • the powder material mixed with copper oxide or yttrium oxide may have a powder resistance of less than (1.00E + 4) ⁇ , and sufficient electrical conductivity cannot be expected to be achieved. ..
  • the powder material to which aluminum oxide or titanium oxide is added and mixed can produce a copper laminated model having a powder resistance of (1.00E + 4) ⁇ or more and an electric conductivity of 60% IACS or more.
  • the powder resistance is (1.00E + 4) ⁇ or more and the electrical conductivity is 60% IACS or more regardless of the powder material to which any nanooxide is added and mixed. It can be seen that the copper laminated model can be produced.
  • the copper laminated model can be obtained as in the case of SiO 2 . It can be expected that an electric conductivity of 80% IACS or more, which is a pure copper product, can be achieved.
  • a powder bed can be formed and the laminated molding copper containing the pure copper powder can be formed.
  • the powder resistance value of the powder is in the range of (7.50E + 5) ⁇ to (2.50E + 7) ⁇ .
  • a powder bed can be formed, and the relative density is 99% or more when melted at the energy density of the existing equipment.
  • a copper laminated model can be produced, but the electrical conductivity of the copper laminated model does not exceed 80% IACS, which is a pure copper product.
  • nanosilica (SiO 2 ) was used as the nanooxide to be added and mixed, but the energy density of the existing apparatus was reduced by reducing the powder resistance from the pure copper powder having an average particle size of 20 ⁇ m or less.
  • Any nanooxide may be used as long as it can be melted in the above and the fluidity can be improved to form a powder bed with an existing device.
  • any nanooxide may be used as long as the density of the pure copper laminated model produced by the laminated modeling device is 99% or more and the electric conductivity is 80% IACS or more.
  • the shape and particle size of the nanooxide are also preferably selected.

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WO2023047044A1 (fr) * 2021-09-27 2023-03-30 Addup Procédé de fabrication additive d'un objet en cuivre
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