WO2017100174A1 - Procédés de fabrication de composites à matrice métallique comprenant des particules inorganiques et des fibres discontinues - Google Patents

Procédés de fabrication de composites à matrice métallique comprenant des particules inorganiques et des fibres discontinues Download PDF

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Publication number
WO2017100174A1
WO2017100174A1 PCT/US2016/065101 US2016065101W WO2017100174A1 WO 2017100174 A1 WO2017100174 A1 WO 2017100174A1 US 2016065101 W US2016065101 W US 2016065101W WO 2017100174 A1 WO2017100174 A1 WO 2017100174A1
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Prior art keywords
particles
metal
porous
metal matrix
matrix composite
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Ceased
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PCT/US2016/065101
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English (en)
Inventor
Elizaveta Y. PLOTNIKOV
Douglas E. Johnson
Colin Mccullough
Jason D. ANDERSON
Gang Qi
Yong K. Wu
Sandeep K. Singh
Gareth A. Hughes
David M. Wilson
Anatoly Z. Rosenflanz
Douglas P. Goetz
Jordan A. CAMPBELL
Fabian STOLZENBURG
Jean A. Tangeman
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3M Innovative Properties Co
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3M Innovative Properties Co
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Priority to US15/781,670 priority Critical patent/US20180272428A1/en
Priority to EP16873665.0A priority patent/EP3386663A4/fr
Priority to KR1020187018919A priority patent/KR20180091865A/ko
Priority to CN201680072891.9A priority patent/CN108367358A/zh
Publication of WO2017100174A1 publication Critical patent/WO2017100174A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04—Light metals
    • C22C49/06—Aluminium
    • 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
    • B22F3/11—Making porous workpieces or articles
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • B22F3/1112—Making porous workpieces or articles with particular physical characteristics comprising hollow spheres or hollow fibres
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • B22F3/1118—Making porous workpieces or articles with particular physical characteristics comprising internal reinforcements
    • 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
    • B22F7/002—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 porous nature
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • 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
    • C22C32/0089—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 other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04—Light metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • B22F2003/1106—Product comprising closed porosity
    • 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
    • B22F2301/05—Light metals
    • B22F2301/052—Aluminium
    • 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
    • B22F2301/05—Light metals
    • B22F2301/058—Magnesium

Definitions

  • the present disclosure relates to methods of making metal matrix composites, which include a mixture of a metal base with other materials, such as filler materials.
  • Metal matrix composites have long been recognized as promising materials due to their combination of high strength and stiffness combined with low weight.
  • Metal matrix composites typically include a metal matrix reinforced with fibers or other filler materials.
  • the present disclosure provides methods for making a lightweighted metal matrix composite. There remains a need for methods of forming metal matrix composites that have a lower envelope density than the metal while maintaining certain levels of physical properties.
  • the present disclosure provides a method of making a porous metal matrix composite.
  • the method includes mixing a metal powder, a plurality of inorganic particles, and a plurality of discontinuous fibers, thereby forming a mixture.
  • the method further includes sintering the mixture, thereby forming the porous metal matrix composite.
  • the inorganic particles and the discontinuous fibers are dispersed in the metal.
  • An advantage of at least one exemplary embodiment of the present disclosure is that a porous metal matrix composite is manufactured, the metal matrix composite containing inorganic particles and discontinuous fibers dispersed in metal exhibiting both a lower envelope density than the metal and an acceptable yield strength (e.g., plastic yielding in a tensile stress-strain curve). Moreover, it is not necessary to use any coating on the inorganic particles to provide metal matrix composites having inorganic particles effectively dispersed in the metal, according to at least some exemplary embodiments of the present disclosure. The inorganic particles are typically intact within the metal matrix composite, with minimal broken particles in at least some exemplary embodiments of the present disclosure.
  • Figure 1 is a schematic cross-section view of a metal matrix composite manufactured according to an exemplary embodiment of the present disclosure.
  • Figure 2 is a graph of stress-strain curves for exemplary and comparative matrices prepared according to the present disclosure.
  • Figure 3 is a graph of stress-strain curves for additional exemplary matrices and comparative matrices.
  • Figure 4 is a graph of stress-strain curves for further exemplary matrices and comparative matrices.
  • Figure 5 is a graph of stress-strain curves for another exemplary matrix.
  • Figure 6 is a graph of stress-strain curves for still further exemplary matrices.
  • Figure 7 is a graph of stress-strain curves for yet another exemplary matrix.
  • the term "dispersed" with respect to one or more fillers in a metal matrix refers to the one or more fillers distributed throughout the metal matrix, for instance providing a substantially homogeneous metal matrix composite including the metal and the filler(s). This is in contrast to areas of a metal matrix composite having a concentration of one or more fillers that is at least twice as high as an area in a different location of the metal matrix composite (e.g., layers or clusters of a filler within the metal matrix composite). Although it may be possible to observe a sufficiently small volume of a metal matrix composite in which the one or more fillers is not exactly homogenously distributed in the metal matrix, the filler(s) is still dispersed in the metal.
  • sinter refers to making a powdered material coalesce into a solid or porous mass by heating it without complete liquefaction. Optionally, the powdered material is also compressed during sintering.
  • envelope density refers to the mass divided by the envelope volume.
  • envelope volume refers to the sum of the volumes of the solid in each particle and any voids in the particle.
  • envelope density refers to the mass divided by the envelope volume, where the “envelope volume” refers to the sum of the volumes of the solid in the metal matrix composite and any voids in the metal matrix composite.
  • skeleton density with respect to porous particles refers to the mass divided by the skeleton volume.
  • skeleton volume refers to the sum of the volumes of the solid material and any closed pores within the particle.
  • average true density refers to the mean of the density of the glass bubbles rather than the density of a volume of glass bubbles (which is dependent on compaction of the glass bubbles in that volume).
  • plastic yield refers to the stress at which a predetermined amount of permanent deformation of a material occurs.
  • tensile plastic yield refers to the stress at which a predetermined amount of permanent deformation of a material occurs while the material is being subjected to a tensile force.
  • the term "softening point” refers to the temperature, or range of temperatures, at which a material (e.g., in a solid phase) begins to slump under its own weight.
  • the softening point is generally regarded as being the melting point of the metal or metal alloy.
  • the softening point may be the temperature at which elastic behavior of the material changes to plastic flow.
  • the softening point of a glass, a glass-ceramic, or a porcelain may occur at a glass-transition temperature of the material, and may be defined by a viscosity of 10 7 65 poise.
  • the softening point of glass is typically determined, for example, by the Vicat method (e.g., ASTM-D1525 or ISO 306) or by the Heat Deflection Test (e.g., ASTM-D648).
  • uncoated with respect to glass bubbles refers to the absence of any additional material (i.e., having a composition different from the glass) applied to an exterior surface of the glass bubbles.
  • yield strength refers to the stress at which it is considered that plastic elongation of a material has commenced. As used herein, the yield strength is determined at an offset of 0.2%. ASTM B557M-15 discloses "7.6 Yield Strength— Determine yield strength by the offset method at an offset of 0.2 %. Acceptance or rejection of material may be decided on the basis of Extension-Under-Load Method. For referee testing, the offset method shall be used. 7.6.1 Offset Method— To determine the yield strength by the "offset method,” it is necessary to secure data (autographic or numerical) from which a stress-strain diagram may be drawn. Then on the stress-strain diagram (Fig.
  • transitional-alumina refers to any alumina from aluminum hydroxide to alpha-alumina.
  • Specific transitional-alumina particles include delta-alumina, eta-alumina, theta- alumina, chi-alumina, kappa-alumina, rho-alumina, and gamma-alumina.
  • the transitional-alumina particles are generated during the heat treatment of aluminum hydroxide or aluminum oxy hydroxide.
  • the most thermodynamically stable form is generally alpha-alumina.
  • the present disclosure provides a method of making a porous metal matrix composite.
  • the method includes mixing a metal powder, a plurality of inorganic particles, and a plurality of discontinuous fibers to form a mixture.
  • the method further includes sintering the mixture to form the porous metal matrix composite.
  • mixing of the metal powder, inorganic particles, and discontinuous fibers is performed manually, such as by shaking by hand a container holding the materials. Often, shaking is performed for at least 15 seconds, at least 20 seconds, at least 30 seconds, at least 45 seconds, or at least 60 seconds, and up to 2 minutes, up to 100 seconds, up to 90 seconds, or up to 70 seconds.
  • a container holding the materials is inverted at least once.
  • mixing of the metal powder, inorganic particles, and discontinuous fibers is performed using an acoustic mixer, a mechanical mixer, a shaker table, or a tumbler.
  • Mixing using an apparatus may similarly be performed for at least 15 seconds, at least 20 seconds, at least 30 seconds, at least 45 seconds, or at least 60 seconds, and up to 2 minutes, up to 100 seconds, up to 90 seconds, or up to 70 seconds.
  • the mixture created by mixing the components comprises the inorganic particles and the discontinuous fibers dispersed in the metal powder. As discussed above, having the inorganic particles and discontinuous fibers dispersed in the metal powder provides a substantially homogeneous mixture.
  • the mixture is sintered.
  • the sintering is performed for a time of at least 30 minutes, at least 60 minutes, at least 90 minutes, or at least 2 hours, and up to 3 hours or up to 24 hours; such as between 30 minutes and 3 hours, inclusive.
  • the mixture is sintered in a die (e.g., a mold).
  • the sintering is usually performed in a hot press or a furnace at a temperature of at least 250 degrees Celsius (°C), at least 300 °C, at least 400 °C, at least 500 °C, or at least 600 °C, and up to 1,000 °C, up to 900 °C, up to 800 °C, or up to 700 °C; such as between 250 °C and 1,000 °C, inclusive, or between 400 °C and 900 °C , or between 600 °C and 800 °C.
  • the temperature is increased at a steady rate until a desired maximum temperature is reached.
  • the sintering further comprises applying pressure to the mixture in the die.
  • sintering is optionally performed at a pressure of at least 4 megapascals (MPa), at least 5 MPa, at least 7 MPa, at least 10 MPa, at least 12 MPa, at least 15 MPa, or at least 20 MPa; and up to 200 MPa, up to 150 MPa, up to 100 MPa, up to 75 MPa, up to 50 MPa, or up to 25 MPa; such as between 4 MPa and 200 MPa, inclusive, between 4 MPa and 50 MPa, inclusive, or between 15 MPa and 200 MPa, inclusive.
  • the die is flushed with an inert gas (e.g., nitrogen or argon) following the release of applied pressure.
  • an inert gas e.g., nitrogen or argon
  • the metal matrix composite can be allowed to cool (e.g., within or outside the hot press or furnace).
  • the metal matrix composite is allowed to furnace cool (i.e., by turning off the furnace and waiting for the metal matrix composite to cool down on its own).
  • a coolant for instance and without limitation, an inert gas (e.g., nitrogen, argon, etc.), is passed through the hot press or furnace to help the metal matrix composite to cool down faster.
  • an inert gas e.g., nitrogen, argon, etc.
  • the porous metal matrix composite 100 includes a metal 10, a plurality of inorganic particles 12, and a plurality of discontinuous fibers 14.
  • the inorganic particles 12 and the discontinuous fibers 14 are dispersed in the metal 10.
  • the metal matrix composite is illustrated as having a monolithic shape; however, the metal matrix composite may be formed in a number of various shapes depending on the intended application.
  • Metal matrix composites are applicable to industries such as construction, automotive, and electronics, in which a particular metal component may be replaced with a metal matrix composite component.
  • the metal comprises a porous matrix structure.
  • a porous matrix structure is usually obtained from powdered metal, wherein the powder contains a metal structure in which a gas (e.g., air) is incorporated into the solid metal structure.
  • a gas e.g., air
  • the metal is present in an amount of 50 weight percent or more of the metal matrix composite, 55 weight percent or more, 60 weight percent or more, 65 weight percent or more, 70 weight percent or more, or 75 weight percent or more; and in an amount of 95 weight percent or less, 90 weight percent or less, 85 weight percent or less, or 80 weight percent or less.
  • the metal may be present in an amount of between 50 weight percent and 95 weight percent, inclusive, of the metal matrix composite, or between 70 weight percent and 95 weight percent, inclusive, of the metal matrix composite.
  • the metal comprises aluminum, magnesium, or alloys thereof (i.e., an aluminum alloy or a magnesium alloy). Suitable metals include for instance and without limitation, pure aluminum (aluminum powder with purity of at least 99.0%, e.g., AA1100, AA1050, AA1070 etc. , such as pure aluminum powder commercially available from Eckart (Louisville, KY)); or an aluminum alloy containing aluminum and 0.2 to 2% by mass of another metal.
  • Such alloys include: Al— Cu alloys (AA2017 etc.), Al— Mg alloys (AA5052 etc.), Al— Mg— Si alloys (AA6061 etc.), Al— Zn— Mg alloys (AA7075 etc.) and Al— Mn alloys, either alone or as a mixture of two or more.
  • Various suitable metal powders are commercially available from Atlantic Equipment Engineers (Upper Saddle River, NJ).
  • the metal powder comprises an average particle size of 300 nanometers (nm) or more, 400 nm or more, 500 nm or more, 750 nm or more, 1 micrometer ( ⁇ ) or more, 2 ⁇ or more, 5 ⁇ or more, 7 ⁇ or more, 10 ⁇ or more, 20 ⁇ or more, 35 ⁇ or more, 50 ⁇ or more, or 75 ⁇ or more; and 100 ⁇ or less, 75 ⁇ or less, 50 ⁇ or less, 35 ⁇ or less, or 25 ⁇ or less.
  • the metal powder comprises an average particle size ranging between 300 nm and 100 ⁇ , inclusive; ranging between 1 ⁇ and 100 ⁇ , inclusive; or ranging between 1 ⁇ and 50 ⁇ , inclusive.
  • the particle size can be analyzed, for instance, using light microscopy and laser diffraction.
  • Suitable inorganic particles include particles having a maximum envelope density of 2.00 grams per cubic centimeter or less, 1.75 grams per cubic centimeter or less, 1.50 grams per cubic centimeter or less, 1.25 grams per cubic centimeter or less, or 1.00 grams per cubic centimeter or less.
  • the plurality of inorganic particles comprises a substantially spherical shape or an acicular shape, while in some embodiments the inorganic particles comprise multicelled bubbles.
  • the particles generally have an aspect ratio of longest axis to shortest axis of 2 : 1 or less.
  • the plurality of inorganic particles comprises an average particle size of 50 nanometers (nm) or more, 250 nm or more, 500 nm or more, 750 nm or more, 1 micrometer ( ⁇ ) or more, 2 ⁇ or more, 5 ⁇ or more, 7 ⁇ or more, 10 ⁇ or more, 20 ⁇ or more, 35 ⁇ or more, 50 ⁇ or more, 75 ⁇ or more, or 100 ⁇ or more; and 5 millimeters (mm) or less, 3 mm or less, 2 mm or less, 1 mm or less, 750 ⁇ or less, 500 ⁇ or less, or 250 ⁇ or less.
  • the plurality of inorganic particles comprises an average particle size ranging between 50 nm and 5 mm, inclusive; ranging between 1 ⁇ and 1 mm, inclusive; or ranging between 10 ⁇ and 500 ⁇ , inclusive.
  • the amount of inorganic particles dispersed in the metal is not particularly limited.
  • the plurality of inorganic particles is often present in an amount of at least 1 weight percent of the metal matrix composite, at least 2 weight percent, at least 5 weight percent, at least 8 weight percent, at least 10 weight percent, at least 15 weight percent, or at least 20 weight percent of the metal matrix composite; and up to 50 weight percent, up to 28 weight percent, up to 26 weight percent, up to 24 weight percent, or up to 22 weight percent of the metal matrix composite.
  • the inorganic particles are present in the metal matrix composite in an amount of between 1 weight percent and 30 weight percent, or between 2 weight percent and 25 weight percent, or between 2 weight percent and 15 weight percent, inclusive, of the metal matrix composite.
  • Including less than 1 weight percent of the inorganic particles results in a minimal decrease in envelope density of the metal matrix composite, while including more than 30 weight percent of the inorganic particles negatively impacts the mechanical properties of the metal matrix composite due to the metal matrix composite containing an insufficient amount of metal and fibers.
  • the plurality of inorganic particles comprise porous particles.
  • porous particles refers to both particles that have pores themselves, and agglomerates of nonporous primary particles including pores between at least some of the nonporous primary particles.
  • useful porous particles include for instance and without limitation, porous metal oxide particles, porous metal hydroxide particles, porous metal carbonates, porous carbon particles, porous silica particles, porous dehydrated aluminosilicate particles, porous dehydrated metal hydrate particles, zeolite particles, porous glass particles, expanded perlite particles, expanded vermiculite particles, porous sodium silicate particles, engineered porous ceramic particles, agglomerates of nonporous primary particles, or
  • the metal of the metal oxide, metal hydroxide, or metal carbonate is selected from aluminum, magnesium, zirconium, calcium, or combinations thereof.
  • the porous particles comprise porous alumina particles, porous carbon particles, porous silica particles, porous aluminum hydroxide particles, or combinations thereof.
  • the porous particles typically have had associated water removed from them, usually by heating the porous particles.
  • the porous particles comprise transitional-alumina particles. Suitable porous particles include for instance and without limitation, Versal 250 boehmite powder commercially available from UOP LLC (Des Plaines, IL), YH-D 16 boehmite powder, Zibo Yinghe Chemical Company, Ltd. (Shandong, China), and Alumax PB300 boehmite, PIDC International (Ann Arbor, MI).
  • the plurality of inorganic particles comprises ceramic bubbles or glass bubbles.
  • Suitable materials for ceramic bubbles and glass bubbles includes, for instance and without limitation, alumina, aluminosilicate, silica, or combinations thereof.
  • Commercially available glass bubbles include, for example, the LightStar, EconoStar, and High Alumina censopheres available from Cenostar Corporation (Amesbury, MA).
  • the ceramic bubbles and glass bubbles are uncoated (e.g., with a metal material, which has been used to aid in wetting of the bubbles by the metal matrix).
  • the plurality of (e.g., uncoated) glass bubbles advantageously comprises glass that withstands heating to a temperature of 700 degrees Celsius for at least two hours without softening.
  • the use of high temperature resistant glass bubbles allows their incorporation in metal matrix composites that otherwise would be prepared at a temperature elevated enough to damage the glass bubbles, such as by softening at least some of the glass bubbles to the point that they deform and/or break.
  • One suitable type of glass bubbles includes bubbles that leach less than 100 micrograms of sodium ion per gram of glass bubbles in deionized water when stirred with the deionized water for 2 hours.
  • An advantage of glass bubbles with such a low sodium leaching rate is that they are useful in electronics applications where the leaching of sodium ions is often unacceptable.
  • suitable compounds used for the preparation of such low sodium glass bubbles include silica, lime, boric acid, calcium phosphate, calcined alumina silicate, and magnesium silicate.
  • such low sodium glass bubbles exhibit a softening temperature between 717 °C and 735 °C, inclusive, as measured by thermal dilatometry.
  • the inorganic particles comprise uncoated inorganic particles.
  • employing uncoated inorganic particles provides a savings in material costs and coating time.
  • Methods according to at least certain embodiments of the present disclosure prepare porous metal matrix composites in which the inorganic particles are dispersed in the metal without requiring any further material to improve contact between the inorganic particles and the metal.
  • the plurality of discontinuous fibers dispersed in the metal matrix composite is not particularly limited, and for example includes inorganic fibers, such as glass, alumina, aluminosilicate, carbon, basalt, or a combination thereof. More particularly, in certain embodiments the fibers comprise at least one metal oxide, alumina, alumina-silica, or a combination thereof.
  • the discontinuous fibers have an average length of less than 5 centimeters, which tend to be more conducive to dispersion in a metal matrix than longer fibers. In many embodiments, the fibers have an average length that is shorter than the smallest dimension of the mold or die used to form a metal matrix composite, so that the orientation of the fibers is not restricted by the mold or die.
  • a ratio of the fiber length to the smallest dimension of the mold or die is ⁇ 1 : 1.
  • the discontinuous fibers have an average length of less than 4 centimeters, less than 3 centimeters, or less than 2 centimeters.
  • Discontinuous fibers may be formed from continuous fibers, for example, by methods known in the art such as chopping and milling.
  • the plurality of discontinuous fibers comprises an aspect ratio of 10 : 1 or greater.
  • Suitable discontinuous fibers can have a variety of compositions, such as ceramic fibers.
  • the ceramic fibers can be produced in continuous lengths, which are chopped or sheared, as discussed herein, to provide the ceramic fibers of the present disclosure.
  • the ceramic fibers can be produced from a variety of commercially available ceramic filaments. Examples of filaments useful in forming the ceramic fibers include the ceramic oxide fibers sold under the trademark NEXTEL (3M Company, St. Paul, MN). NEXTEL is a continuous filament ceramic oxide fiber having low elongation and shrinkage at operating temperatures, and offers good chemical resistance, low thermal conductivity, thermal shock resistance, and low porosity.
  • NEXTEL fibers include NEXTEL 312, NEXTEL 440, NEXTEL 550, NEXTEL 610 and NEXTEL 720.
  • NEXTEL 312 and NEXTEL 440 are refractory aluminoborosilicate that includes A1 2 0 3 , Si0 2 and B 2 0 3 .
  • NEXTEL 550 and NEXTEL 720 are aluminosilica and NEXTEL 610 is alumina.
  • the NEXTEL filaments are coated with organic sizings or finishes which serves as aids in textile processing.
  • Sizing can include the use of starch, oil, wax or other organic ingredients applied to the filament strand to protect and aid handling.
  • the sizing can be removed from the ceramic filaments by heat cleaning the filaments or ceramic fibers as a temperature of 700 °C for one to four hours.
  • the ceramic fibers can be cut or chopped so as to provide relatively uniform lengths, which can be accomplished by cutting continuous filaments of the ceramic material in a mechanical shearing operation or laser cutting operation, among other cutting operations. Given the highly controlled nature of such cutting operations, the size distribution of the ceramic fibers is very narrow and allow to control the composite property.
  • the length of the ceramic fiber can be determined, for instance, using an optical microscope (Olympus MX61, Tokyo, Japan) fit with a CCD Camera (Olympus DP72, Tokyo, Japan) and analytic software (Olympus Stream Essentials, Tokyo, Japan). Samples may be prepared by spreading representative samplings of the ceramic fiber on a glass slide and measuring the lengths of at least 200 ceramic fibers at 10X magnification.
  • Suitable fibers include for instance ceramic fibers available under the trade name NEXTEL (available from 3M Company, St. Paul, MN), such as NEXTEL 312, 440, 610 and 720.
  • NEXTEL available from 3M Company, St. Paul, MN
  • One presently preferred ceramic fiber comprises polycrystalline (X-AI2O3.
  • Suitable alumina fibers are described, for example, in U.S. Pat. No. 4,954,462 (Wood et al.) and U.S. Pat. No. 5, 185,299 (Wood et al).
  • Exemplary alpha alumina fibers are marketed under the trade designation NEXTEL 610 (3M Company, St. Paul, MN).
  • the alumina fibers are polycrystalline alpha alumina fibers and comprise, on a theoretical oxide basis, greater than 99 percent by weight AI2O3 and 0.2-0.5 percent by weight S1O2, based on the total weight of the alumina fibers.
  • some desirable polycrystalline, alpha alumina fibers comprise alpha alumina having an average grain size of less than one micrometer (or even, in some embodiments, less than 0.5 micrometer).
  • polycrystalline, alpha alumina fibers have an average tensile strength of at least 1.6 GPa (in some embodiments, at least 2.1 GPa, or even, at least 2.8 GPa).
  • Suitable aluminosilicate fibers are described, for example, in U.S. Pat. No. 4,047,965 (Karst et al). Exemplary aluminosilicate fibers are marketed under the trade designations NEXTEL 440, and NEXTEL 720, by 3M Company (St. Paul, MN). Aluminoborosilicate fibers are described, for example, in U.S. Pat. No. 3,795,524 (Sowman). Exemplary aluminoborosilicate fibers are marketed under the trade designation NEXTEL 312 by 3M Company. Boron nitride fibers can be made, for example, as described in U.S. Pat. No. 3,429,722 (Economy) and U.S. Pat. No.
  • Ceramic fibers can also be formed from other suitable ceramic oxide filaments.
  • Ceramic oxide filaments examples include those available from Central Glass Fiber Co., Ltd. (e.g., EFH75-01, EFH150-31). Also preferred are aluminoborosilicate glass fibers which are which contain less than about 2% alkali or are substantially free of alkali (i.e., "E-glass" fibers). E-glass fibers are available from numerous commercial suppliers.
  • the amount of discontinuous fibers dispersed in the metal matrix composite is not particularly limited.
  • the plurality of fibers is often present in an amount of at least 1 weight percent of the metal matrix composite, at least 2 weight percent, at least 3 weight percent, at least 5 weight percent, at least 10 weight percent, at least 15 weight percent, at least 20 weight percent, or at least 25 weight percent of the metal matrix composite; and up to 50 weight percent, up to 45 weight percent, up to 40 weight percent, or up to 35 weight percent of the metal matrix composite.
  • the fibers are present in the metal matrix composite in an amount of between 1 weight percent and 50 weight percent, or between 2 weight percent and 25 weight percent, or between 5 weight percent and 15 weight percent, inclusive, of the metal matrix composite.
  • Including less than 1 weight percent of the fibers results in a minimal increase in strength of the metal matrix composite, while including more than 50 weight percent of the fibers negatively impacts the envelope density of the metal matrix composite due to the metal matrix composite containing an insufficient amount of metal and inorganic particles.
  • the plurality of inorganic particles and the plurality of discontinuous fibers are present in combination in an amount of between 5 weight percent and 50 weight percent, inclusive, of the metal matrix composite.
  • the metal matrix composite exhibits both a decreased envelope density (as compared to the pure metal) and acceptable mechanical properties.
  • the metal matrix composite typically has an envelope density between 1.35 and 2.70 grams per cubic centimeter, inclusive or between 1.80 and 2.50 grams per cubic centimeter, inclusive.
  • the metal matrix composite may have an envelope density of at least 1.60 grams per cubic centimeter, at least 1.75, at least 1.90, at least 2.00, at least 2.10, or at least 2.25 grams per cubic centimeter; and an envelope density of up to 2.70, up to 2.60, up to 2.50, up to 2.40, or up to 2.30 grams per cubic centimeter.
  • the metal comprises aluminum or alloys thereof and the metal matrix composite has an envelope density between 1.80 and 2.50 grams per cubic centimeter, inclusive; between 2.00 and 2.30 grams per cubic centimeter, inclusive; or between 1.80 and 2.20 grams per cubic centimeter, inclusive.
  • the metal comprises magnesium or alloys thereof and the metal matrix composite has an envelope density between 1.35 and 1.60 grams per cubic centimeter, inclusive; between 1.55 and 1.60 grams per cubic centimeter, inclusive; or between 1.35 and 1.50 grams per cubic centimeter, inclusive.
  • the metal matrix composite has an envelope density that is at least 8% less than the density of the metal (or at least 10% less, at least 12% less, at least 15% less, or at least 17% less) and can withstand a strain of 1% prior to fracture. This combination of properties provides both lightweighting of the metal and maintains some of the metal characteristics in the metal matrix composite.
  • the metal matrix composite preferably exhibits a yield strength before failure in a tensile test.
  • the metal matrix composite has a yield strength of 50 megapascals or greater, 75 megapascals or greater, 100 megapascals or greater, 150 megapascals or greater, or 200 megapascals or greater.
  • the metal matrix composite of at least certain exemplary embodiments of the present disclosure exhibits a stress-strain curve that shows a plastic yielding behavior
  • the metal matrix composite of at least certain exemplary embodiments of the present disclosure exhibits a stress-strain curve that shows a tensile plastic yield behavior. That is to say, that the stress-strain curve exhibits a region of plastic flow.
  • the plastic yield curve and tensile plastic yield curve are in contrast to a purely brittle failure mechanism. That is to say, the purely brittle behavior exhibits only an elastic region within the stress-strain curve, and no (or very little) region of plastic flow.
  • the combination of both inorganic particles and discontinuous fibers as fillers in metal matrix composites provided a plastic yield curve and/or a tensile plastic yield behavior upon testing.
  • a plastic yield curve and/or a tensile plastic yield behavior upon testing For instance, referring to FIG. 3, the stress-strain curve for Example 13, containing both fibers and porous inorganic particles (described in detail below), shows a yield before a brittle failure mechanism.
  • the metal matrix composite can withstand a strain of 1%, 1.5%, or 2% prior to fracture.
  • the metal powder remained separate from the porous inorganic particles, as opposed to being pushed into some of the pores of the porous inorganic particles during sintering (particularly sintering under applied pressure).
  • the porous inorganic particles further, interestingly, did not tend to become damaged (e.g., crumble or crush) during sintering, but rather maintained their porous skeletal structures.
  • the metal matrix composite exhibits an ultimate tensile strength of 25 megapascals (MPa) or greater, such as 40 MPa or greater, 50 MPa or greater, 75 MPa or greater, 100 MPa or greater, 150 MPa or greater, 200 MPa or greater, 250 MPa or greater, or 300 MPa or greater. It can further be useful to consider the tensile strength of a metal matrix composite as it relates to the envelope density of the metal matrix composite as typically tensile strength is sacrificed during lightweighting of a composite.
  • MPa megapascals
  • the metal matrix composite has an envelope density between 1.80 and 2.50 grams per cubic centimeter, inclusive, and an ultimate tensile strength of 50 MPa or greater, 100 MPa or greater, 150 MPa or greater, 200 MPa or greater, 250 MPa or greater, or 300 MPa or greater.
  • desirable mechanical properties are obtained without requiring fillers beyond the inorganic particles and the discontinuous fibers.
  • the metal matrix composite consists essentially of a metal, a plurality of inorganic particles, and a plurality of discontinuous fibers.
  • the metal matrix composite thus may further contain additives that do not substantially impact the mechanical properties of the metal matrix composite.
  • a metal matrix composite consisting essentially of a metal, a plurality of inorganic particles, and a plurality of discontinuous fibers could not further include additives such as materials used to aid dispersion of the fillers.
  • Metal matrix composites according to aspects of the present disclosure can be prepared according to various suitable methods known to the skilled practitioner, including powder metallurgy processes such as hot pressing, powder extrusion, hot rolling, heating followed by warm rolling, cold compaction and sintering, and hot isostatic pressing.
  • the metal matrix composites may be prepared by mixing a metal powder, the plurality of inorganic particles, and the plurality of discontinuous fibers to disperse the inorganic particles and discontinuous fibers in the metal powder, followed by sintering of the mixture to form a metal matrix composite.
  • powder metallurgy method is described in detail below in Example 1.
  • Embodiment 1 is a method of making a porous metal matrix composite.
  • the method includes mixing a metal powder, a plurality of inorganic particles, and a plurality of discontinuous fibers, thereby forming a mixture.
  • the method further includes sintering the mixture, thereby forming the porous metal matrix composite.
  • Embodiment 2 is the method of embodiment 1, wherein the mixture is sintered in a die.
  • Embodiment 3 is the method of embodiment 1 or embodiment 2, wherein the sintering is performed at a temperature of between 250 degrees Celsius and 1,000 degrees Celsius, inclusive.
  • Embodiment 4 is the method of any of embodiments 1 to 3, wherein the sintering comprises applied pressure.
  • Embodiment 5 is the method of embodiment 4, wherein the sintering is performed at a pressure of between 4 megapascals and 200 megapascals, inclusive.
  • Embodiment 6 is the method of any of embodiments 1 to 5, wherein the sintering is performed for a time of between 30 minutes and 3 hours, inclusive.
  • Embodiment 7 is the method of any of embodiments 1 to 6, wherein the mixing is performed using an acoustic mixer, a mechanical mixer, or a tumbler.
  • Embodiment 8 is the method of any of embodiments 1 to 7, wherein the mixture comprises the inorganic particles and the discontinuous fibers dispersed in the metal powder.
  • Embodiment 9 is the method of any of embodiments 1 to 8, wherein the metal matrix composite has an envelope density that is at least 8% less than the density of the metal and can withstand a strain of 1% prior to fracture.
  • Embodiment 10 is the method of embodiment 9, wherein the metal matrix composite can withstand a strain of 2% prior to fracture.
  • Embodiment 11 is the method of any of embodiments 1 to 10, wherein the metal matrix composite has a yield strength of 50 megapascals or greater.
  • Embodiment 12 is the method of any of embodiments 1 to 11, wherein the metal matrix composite has a yield strength of 100 megapascals or greater.
  • Embodiment 13 is the method of any of embodiments 1 to 12, wherein the metal matrix composite has an ultimate tensile strength of 100 megapascals or greater.
  • Embodiment 14 is the method of any of embodiments 1 to 13, wherein the metal matrix composite has an ultimate tensile strength of 200 megapascals or greater.
  • Embodiment 15 is the method of any of embodiments 1 to 14, wherein the metal matrix composite has an ultimate tensile strength of 300 megapascals or greater.
  • Embodiment 16 is the method of any of embodiments 1 to 15, wherein the plurality of inorganic particles comprises porous particles.
  • Embodiment 17 is the method of embodiment 16, wherein the porous particles have a maximum envelope density of 2 grams per cubic centimeter or less.
  • Embodiment 18 is the method of embodiment 15 or embodiment 16, wherein the porous particles comprise porous metal oxide particles, porous metal hydroxide particles, porous metal carbonates, porous carbon particles, porous silica particles, porous dehydrated
  • Embodiment 19 is the method of any of embodiments 16 to 18, wherein the porous particles comprise porous alumina particles, porous carbon particles, porous silica particles, porous aluminum hydroxide particles, or combinations thereof.
  • Embodiment 20 is the metal matrix composite of embodiment 19, wherein the porous particles comprise transitional -alumina particles.
  • Embodiment 21 is the method of any of embodiments 1 to 15, wherein the plurality of the inorganic particles comprise ceramic bubbles or glass bubbles.
  • Embodiment 22 is the method of embodiment 21, wherein the glass bubbles comprise glass that withstands heating to a temperature of 700 degrees Celsius for at least two hours without softening.
  • Embodiment 23 is the method of embodiment 21 or embodiment 22, wherein the glass bubbles leach less than 100 micrograms of sodium ion per gram of glass bubbles in deionized water when stirred with the deionized water for 2 hours.
  • Embodiment 24 is the method of any of embodiments 1 to 23, wherein the plurality of inorganic particles comprise a maximum envelope density of 2 grams per cubic centimeter or less.
  • Embodiment 25 is the method of any of embodiments 21 to 23, wherein the plurality of inorganic particles comprises alumina, aluminosilicate, silica, or combinations thereof.
  • Embodiment 26 is the method of any of embodiments 18 to 21, 24, or 25, wherein the inorganic particles comprise multicelled bubbles.
  • Embodiment 27 is the method of any of embodiments 1 to 26, wherein the plurality of inorganic particles has a substantially spherical shape or an acicular shape.
  • Embodiment 28 is the method of any of embodiments 1 to 27, wherein the plurality of inorganic particles has an average particle size ranging between 50 nanometers (nm) and 5 millimeters (mm), inclusive.
  • Embodiment 29 is the method of any of embodiments 1 to 28, wherein the plurality of inorganic particles has an average particle size ranging between 1 micrometer ( ⁇ ) and 1 mm, inclusive.
  • Embodiment 30 is the method of any of embodiments 1 to 29, wherein the plurality of inorganic particles has an average particle size ranging between 10 ⁇ and 500 ⁇ , inclusive.
  • Embodiment 31 is the method of any of embodiments 1 to 30, wherein the plurality of discontinuous fibers comprises glass, alumina, aluminosilicate, carbon, basalt, or a combination thereof.
  • Embodiment 32 is the method of any of embodiments 1 to 31, wherein the plurality of discontinuous fibers has an aspect ratio of 10 : 1 or greater.
  • Embodiment 33 is the method of any of embodiments 1 to 32, wherein the metal comprises a porous matrix structure.
  • Embodiment 34 is method of any of embodiments 1 to 33, wherein the metal comprises aluminum or alloys thereof.
  • Embodiment 35 is the method of any of embodiments 1 to 34, wherein the metal matrix composite has an envelope density between 1.80 and 2.50 grams per cubic centimeter, inclusive.
  • Embodiment 36 is the method of any of embodiments 1 to 34, wherein the metal matrix composite has an envelope density between 2.00 and 2.30 grams per cubic centimeter, inclusive.
  • Embodiment 37 is the method of any of embodiments 1 to 34, wherein the metal matrix composite has an envelope density between 1.80 and 2.20 grams per cubic centimeter, inclusive.
  • Embodiment 38 is the method of any of embodiments 1 to 33, wherein the metal comprises magnesium or alloys thereof.
  • Embodiment 39 is the method of embodiment 38, wherein the metal matrix composite has an envelope density between 1.35 and 1.60 grams per cubic centimeter, inclusive.
  • Embodiment 40 is the method of embodiment 38 or embodiment 39, wherein the metal matrix composite has an envelope density between 1.55 and 1.60 grams per cubic centimeter, inclusive.
  • Embodiment 41 is the method of embodiment 38 or embodiment 39, wherein the metal matrix composite has an envelope density between 1.35 and 1.50 grams per cubic centimeter, inclusive.
  • Embodiment 42 is the method of any of embodiments 1 to 41, wherein the metal matrix composite exhibits a yield strength before failure in a tensile test.
  • Embodiment 43 is the method of any of embodiments 1 to 42, wherein the metal is present in an amount of between 50 weight percent and 95 weight percent, inclusive, of the metal matrix composite.
  • Embodiment 44 is the method of any of embodiments 1 to 43, wherein the plurality of inorganic particles is present in an amount of between 2 weight percent and 50 weight percent, inclusive, of the metal matrix composite.
  • Embodiment 45 is the method of any of embodiments 1 to 44, wherein the plurality of discontinuous fibers is present in an amount of between 2 weight percent and 25 weight percent, inclusive, of the metal matrix composite.
  • Embodiment 46 is the method of any of embodiments 1 to 45, wherein the plurality of inorganic particles and the plurality of discontinuous fibers are present in combination in an amount of between 5 weight percent and 50 weight percent, inclusive, of the metal matrix composite.
  • Embodiment 47 is the method of any of embodiments 1 to 46, wherein the envelope density of the inorganic particles is at least 40% less than the density of the metal.
  • Embodiment 48 is the metal matrix composite of any of embodiments 1 to 47, wherein the envelope density of the inorganic particles is at least 50% less than the density of the metal.
  • Embodiment 49 is the metal matrix composite of any of embodiments 1 to 48, wherein the metal matrix composite consists essentially of the metal; the plurality of inorganic particles; and the plurality of discontinuous fibers.
  • the stress and strain of metal matrix composites was determined using a three-point bend test.
  • a sample was placed lengthwise between two cylindrical supports spaced apart by 32 millimeters (mm).
  • a third loading cylinder suspended from the load cell of the testing apparatus was lowered so as to touch the sample at its midpoint.
  • a software-controlled load frame provided by MTS Systems Corporation (Eden Prairie, MN) fitted with a 100 kilonewton (KN) load cell was used to apply a load to the center of the sample via the middle loading cylinder.
  • KN kilonewton
  • concentration of that ion in the standard was determined using the measured area of each ion. The identity of each ion was achieved through retention matching only.
  • Al 1-511 powder 10 grams (g) was poured into a circular graphite die with 1.5 inch (3.81 centimeter) inner diameter.
  • the Al 1-511 powder was sintered as follows: The die was loaded into an HP50-7010 hot press (Thermal Technology LLC, Santa Rosa, CA), and the setup was pumped down to vacuum. The die was heated from room temperature at 25 degrees Celsius per minute (deg C/min) to 600 degrees Celsius, where it was held for 15 minutes (min). After the 15 min hold at temperature, 640 kilograms (kg) of force (800 pounds per square inch of pressure for this sized die) was applied at 600 degrees Celsius for 1 hour (hr).
  • HP50-7010 hot press Thermal Technology LLC, Santa Rosa, CA
  • the die was heated from room temperature at 25 degrees Celsius per minute (deg C/min) to 600 degrees Celsius, where it was held for 15 minutes (min). After the 15 min hold at temperature, 640 kilograms (kg) of force (800 pounds per square inch of pressure for this sized die) was applied at 600 degrees
  • Table 6 Compositions and mechanical properties of examples.
  • Table 7 Compositions and mechanical properties of examples.
  • Table 8 Compositions and mechanical properties of examples.

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Abstract

L'invention concerne un procédé de fabrication d'un composite à matrice métallique poreux. Le procédé consiste à mélanger une poudre métallique, une pluralité de particules inorganiques, et une pluralité de fibres discontinues pour former un mélange, la poudre métallique comprenant de l'aluminium, du magnésium, un alliage d'aluminium, ou un alliage de magnésium. Le procédé consiste en outre à fritter le mélange pour former le composite à matrice métallique poreux. Normalement, les particules inorganiques comprennent des particules poreuses ou des bulles céramiques ou des bulles de verre, et les particules inorganiques et les fibres discontinues sont dispersées dans le métal. Le composite à matrice métallique présente une densité inférieure à celle du métal et une limite d'élasticité acceptable.
PCT/US2016/065101 2015-12-08 2016-12-06 Procédés de fabrication de composites à matrice métallique comprenant des particules inorganiques et des fibres discontinues Ceased WO2017100174A1 (fr)

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US15/781,670 US20180272428A1 (en) 2015-12-08 2016-12-06 Methods of Making Metal Matrix Composites Including Inorganic Particles and Discontinuous Fibers
EP16873665.0A EP3386663A4 (fr) 2015-12-08 2016-12-06 Procédés de fabrication de composites à matrice métallique comprenant des particules inorganiques et des fibres discontinues
KR1020187018919A KR20180091865A (ko) 2015-12-08 2016-12-06 무기 입자 및 불연속 섬유를 포함하는 금속 매트릭스 복합재의 제조 방법
CN201680072891.9A CN108367358A (zh) 2015-12-08 2016-12-06 制备包括无机颗粒和不连续纤维的金属基体复合材料的方法

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EP3845332A1 (fr) * 2020-01-06 2021-07-07 Rohr, Inc. Revêtements et structures améliorés par rechargement par laser au moyen d'une matière nano-modifiée

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KR20180090867A (ko) 2018-08-13
EP3386663A4 (fr) 2019-06-12
EP3387160A2 (fr) 2018-10-17
WO2017116590A3 (fr) 2017-11-09
CN108699662A (zh) 2018-10-23
KR20180091865A (ko) 2018-08-16
US20180272428A1 (en) 2018-09-27
US20200299815A1 (en) 2020-09-24
CN108367358A (zh) 2018-08-03
TW201733713A (zh) 2017-10-01
EP3386663A1 (fr) 2018-10-17
TW201736621A (zh) 2017-10-16

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