WO2022138505A1 - アルミニウム粉末混合物およびアルミニウム焼結体の製造方法 - Google Patents

アルミニウム粉末混合物およびアルミニウム焼結体の製造方法 Download PDF

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WO2022138505A1
WO2022138505A1 PCT/JP2021/046827 JP2021046827W WO2022138505A1 WO 2022138505 A1 WO2022138505 A1 WO 2022138505A1 JP 2021046827 W JP2021046827 W JP 2021046827W WO 2022138505 A1 WO2022138505 A1 WO 2022138505A1
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powder
aluminum
mass
aluminum alloy
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French (fr)
Japanese (ja)
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純 加藤
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Priority to EP21910650.7A priority Critical patent/EP4269638A4/en
Priority to US18/258,491 priority patent/US20240033819A1/en
Priority to JP2022571410A priority patent/JP7816171B2/ja
Priority to CN202180086808.4A priority patent/CN116648521A/zh
Publication of WO2022138505A1 publication Critical patent/WO2022138505A1/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • 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
    • B22F1/09—Mixtures of metallic powders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • 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
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • 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
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • 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
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/14—Alloys based on aluminium with copper as the next major constituent with silicon
    • 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
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B22F2201/11—Argon
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/20—Use of vacuum
    • 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
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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 an aluminum powder mixture and a method for producing an aluminum sintered body.
  • Aluminum members are widely used as materials for heat exchangers due to their features such as light weight and high thermal conductivity, but in order to further improve heat dissipation characteristics, a complex shape design that enables more efficient heat exchange is possible. And manufacturing is required.
  • the powder metallurgy method since it is possible to manufacture a shape close to the final form (near net shape) depending on the mold, it is possible to give a shape at low cost. There was a problem that sintering was difficult due to the oxide film formed on the aluminum.
  • the binder jet method has been attracting attention as one of the laminated modeling techniques using metal powder.
  • a binder containing a thermosetting resin, a thermoplastic resin, or a photocurable resin is selectively sprayed from a print head onto a metal powder layer, and the metal powder layer is repeatedly laminated to obtain a desired three-dimensional shape.
  • This is a method of obtaining a three-dimensional metal model through the steps of fixing a binder, removing unnecessary powder, degreasing, and sintering after obtaining a metal powder molded body fixed to the metal powder.
  • This binder jet method has merits such as high accuracy, high productivity, and high recyclability of raw material powder as compared with the existing PBF (Powder Bed Fusion) method and DED (Directed Energy Deposition) method.
  • Patent Document 1 As a technique for solving the problem of the oxide film of aluminum, for example, a technique using a preform by pressure molding as described in Patent Document 1 below or a metal injection molding as described in Patent Document 2 is used for baking. A technique for densifying in the molding process before forming is disclosed. Further, a technique for improving the sinterability is disclosed, such as a technique for applying a fine powder having excellent sinterability of about several ⁇ m as described in Patent Document 3. On the other hand, as a conventional technique of a metal injection molding method using a binder, Patent Document 2 and Patent Document 3 disclose a technique for performing metal laminated molding using a binder.
  • Patent Document 1 or Patent Document 2 there is a problem in terms of productivity because it is necessary to fill the mold with pressure. Further, in the technique using fine powder described in Patent Document 3, if aluminum fine powder having a light specific gravity is used, quality deterioration and safety problems due to scattering during filling may be considered. Further, in the above-mentioned binder jet method, it is difficult to apply a high pressure that causes plastic deformation during powder laminating, so it is difficult to apply the sintering method used in conventional mold molding or metal injection molding as it is. Is. Further, since the powder is repeatedly laminated, stable fluidity and filling property are required for the raw material powder, so that it is difficult to apply a fine powder which is greatly affected by aggregation and scattering.
  • the present inventors have studied a sintering technique using aluminum powder, and decided to use a powder obtained by mixing a low melting point aluminum alloy powder with an aluminum powder having a predetermined particle size in a predetermined mass ratio as a raw material powder. I found it. We have found that by using this raw material powder, the sinterability can be improved and high density can be achieved even without pressurization, and the present invention has been reached.
  • the present invention was devised in view of the above circumstances, and it is possible to further promote sintering between aluminum powders, and it is possible to obtain high density and high electrical conductivity of an aluminum sintered body, which is high.
  • the purpose is to provide a technique that makes it possible to obtain thermal conductivity.
  • the aluminum powder mixture according to the present invention 5% by mass or more and 30% by mass of the pure aluminum and the aluminum alloy powder having a lower melting point than the aluminum alloy are added to the starting powder made of pure aluminum or an aluminum alloy.
  • the following is an aluminum powder mixture, and the aluminum alloy powder contains 1 or 2 types of Si and Cu in an amount of 5% by mass or more and 20% by mass or less, and Mg in an amount of 0.2% by mass or more and 2.0% by mass.
  • the balance consists of aluminum and an aluminum alloy with a composition of unavoidable impurities.
  • a liquid phase is first generated from the low melting point aluminum alloy powder at the time of sintering, and the starting powder becomes the starting powder.
  • the liquid phase gets wet and spreads. Since the aluminum alloy powder having a low melting point contains an appropriate amount of Si and Cu, the powder has a lower melting point than the starting powder.
  • the aluminum alloy powder having a lower melting point than the starting powder contains an appropriate amount of Mg to improve the sinterability.
  • the aluminum powder mixture according to one embodiment of the present invention comprises a starting powder made of pure aluminum or an aluminum alloy constituting the aluminum powder mixture, and an aluminum alloy powder having a lower melting point than the pure aluminum and the aluminum alloy. It is preferable that the melting point difference is 40 ° C. or higher.
  • the melting point difference is 40 ° C. or more
  • a liquid phase is generated first from the low melting point aluminum alloy powder at the time of sintering, and the liquid phase is surely wetted and spread with respect to the starting powder. Therefore, the sinterability is improved.
  • the aluminum powder mixture according to one embodiment of the present invention preferably contains Bi in an amount of 0.1% by mass or more and 1.0% by mass or less in the aluminum alloy constituting the aluminum alloy powder.
  • the aluminum powder mixture according to one embodiment of the present invention preferably has a volume-based frequency cumulative 50% diameter (D50) of both the starting powder and the aluminum alloy powder of 12 ⁇ m or more and 50 ⁇ m or less.
  • D50 volume-based frequency cumulative 50% diameter
  • the starting powder and the aluminum alloy powder have a particle size in the above range, segregation of the particles is unlikely to occur, and the packing density of the powder can be increased.
  • an aluminum powder mixture that can maintain the desired shape when it is made into a sintered body by making it possible to make the shrinkage uniform during sintering, suppress unevenness of sintering shrinkage, and accelerate the progress speed during sintering. Can be provided.
  • the concentration of oxygen contained in the starting powder made of pure aluminum or the aluminum alloy and the aluminum alloy powder is 1.0% by mass or less. preferable.
  • the aluminum powder mixture according to one embodiment of the present invention is preferably a raw material powder for powder metallurgy.
  • the aluminum powder mixture according to one embodiment of the present invention is preferably a raw material powder for metal laminate modeling.
  • the above-mentioned aluminum powder mixture is a raw material powder for powder metallurgy, when it is used for powder metallurgy, it is possible to reliably generate a liquid phase first from an aluminum alloy powder having a low melting point at the time of sintering, and the liquid phase has a melting point.
  • a well-shaped sintered body with a high relative density can be obtained by wetting and spreading between the high starting powders.
  • the above-mentioned aluminum powder mixture is a raw material powder for metal laminated molding, when it is used for laminated molding, it is possible to reliably generate a liquid phase first from the aluminum alloy powder having a low melting point at the time of sintering, and the liquid phase becomes It spreads wet between the starting powders having a high melting point, and it is possible to obtain a metal laminated model as a well-shaped sintered body having a high relative density.
  • 5% by mass of the pure aluminum or an aluminum alloy powder having a lower melting point than the aluminum alloy is added to the starting powder made of pure aluminum or an aluminum alloy.
  • An aluminum powder mixture mixed in an amount of 30% by mass or less is used as a raw material powder.
  • the aluminum alloy powder contains at least one or two types of Si and Cu in an amount of 5% by mass or more and 20% by mass or less, Mg in an amount of 0.2% by mass or more and 2.0% by mass, and the balance is composed of aluminum and unavoidable impurities. It is made of an aluminum alloy having.
  • the aluminum powder mixture is used as a raw material powder, and the raw material powder is filled in a mold without pressurization accompanied by plastic deformation of the raw material powder, and is placed in a vacuum atmosphere at a temperature of 580 to 650 ° C. Sinter in a reducing atmosphere or an inert gas atmosphere.
  • the raw material powder is sintered at 580 to 650 ° C, if it is an aluminum powder mixture in which an appropriate amount of low melting point aluminum alloy powder is added to the starting material powder, a liquid phase is generated first from the low melting point aluminum alloy powder and starting. The liquid phase gets wet and spreads with respect to the powder.
  • the low melting point aluminum alloy powder has a lower melting point than the starting powder because it contains an appropriate amount of Si and Cu.
  • the aluminum alloy powder having a lower melting point than the starting powder contains an appropriate amount of Mg, so that the sinterability is improved. Therefore, it is possible to obtain a well-shaped, high relative density, and dense sintered body.
  • (9) In the method for producing an aluminum sintered body according to another embodiment of the present invention, 5 masses of pure aluminum or an aluminum alloy powder having a melting point lower than that of the aluminum alloy is added to the starting powder made of pure aluminum or an aluminum alloy.
  • An aluminum powder mixture mixed in an amount of% or more and 30% by mass or less is used as a raw material powder.
  • the aluminum alloy powder contains at least one or two types of Si and Cu in an amount of 5% by mass or more and 20% by mass or less, Mg in an amount of 0.1% by mass or more and 2.0% by mass, and the balance is composed of aluminum and unavoidable impurities. It is made of an aluminum alloy having.
  • the aluminum powder mixture is used as a raw material powder, and the raw material powder is press-molded using a mold, and then in a vacuum atmosphere, a reducing atmosphere, or an inert gas atmosphere at a temperature of 580 to 650 ° C. Sinter in.
  • the raw material powder is sintered at 580 to 650 ° C, if it is an aluminum powder mixture in which an appropriate amount of low melting point aluminum alloy powder is added to the starting material powder, a liquid phase is generated first from the low melting point aluminum alloy powder and starting. The liquid phase gets wet and spreads with respect to the powder. Since the aluminum alloy powder having a low melting point contains an appropriate amount of Si and Cu, the melting point is surely lower than that of the starting powder. Since the aluminum alloy powder having a lower melting point than the starting powder contains an appropriate amount of Mg, the sinterability after press molding is improved. Therefore, a dense sintered body having a well-shaped shape and a high relative density can be obtained by press molding.
  • the starting powder made of pure aluminum or an aluminum alloy is mixed with the pure aluminum and an aluminum alloy powder having a lower melting point than the aluminum alloy.
  • An aluminum powder mixture mixed by mass% or more and 30% by mass or less is used as a powder raw material.
  • the aluminum alloy powder contains at least one or two types of Si and Cu in an amount of 5% by mass or more and 20% by mass or less, and Mg in an amount of 0.1% by mass or more and 2.0% by mass, and the balance is an unavoidable impurity and aluminum composition. It is made of an aluminum alloy having.
  • the aluminum powder mixture is used as a raw material powder, and a binder containing a thermosetting resin, a thermoplastic resin or a photocurable resin is selectively sprayed onto a metal powder layer from a printhead, and a metal containing the binder is sprayed.
  • a metal powder molded body fixed to a desired three-dimensional shape is obtained, and then a binder is fixed, unnecessary powder is removed, and a degreasing step is performed, and then the temperature is 580 to 650 ° C.
  • the metal powder molded body is sintered in a vacuum atmosphere, a reducing atmosphere, or an inert gas atmosphere.
  • the raw material powder is sintered at 580 to 650 ° C, if it is an aluminum powder mixture in which an appropriate amount of low melting point aluminum alloy powder is added to the starting material powder, a liquid phase is generated first from the low melting point aluminum alloy powder and starting.
  • the liquid phase gets wet and spreads with respect to the powder. Since the aluminum alloy powder having a low melting point contains an appropriate amount of Si and Cu, the melting point is surely lower than that of the starting powder. Since the aluminum alloy powder having a lower melting point than the starting powder contains an appropriate amount of Mg, the sinterability of the metal powder molded body fixed to a desired three-dimensional shape is improved. Therefore, it is possible to obtain a dense sintered body having a well-shaped shape and a high relative density by a metal powder molded body fixed to a desired three-dimensional shape.
  • Bi is contained in 0.1% by mass or more and 1.0% by mass or less in the aluminum alloy constituting the aluminum alloy powder. Is preferable.
  • a liquid phase can be generated first from the aluminum alloy powder having a low melting point and the liquid phase can be supplied between the starting powders.
  • a liquid phase can be generated so that it spreads wet. Since the aluminum alloy powder having a low melting point contains an appropriate amount of Si and Cu, the melting point is surely lower than that of the starting powder, and the wetting and spreading effect of the liquid phase can be surely exhibited. Further, the aluminum alloy powder having a lower melting point than the starting powder contains Mg in an appropriate amount, so that the sinterability is improved. From the above, it is possible to further promote sintering between powders, to achieve high density as an aluminum sintered body, and to obtain a sintered body showing high electrical conductivity and high thermal conductivity. Will be.
  • FIG. 1 shows an example of an aluminum powder mixture and its sintering process according to the first embodiment
  • (a) is a partially enlarged cross-sectional view showing a laminate of an aluminum powder mixture
  • (b) is a heating of the laminate.
  • (c) is an explanatory view showing an outline of the obtained sintered body
  • (d) is an explanatory view showing a state in which the sintered body is finally processed.
  • FIG. 2 shows an example of the process of sintering an aluminum powder mixture
  • (a) is an explanatory diagram showing an aluminum powder mixture before sintering
  • (b) shows a state in which the liquid phase is wet and spread during sintering.
  • FIG. 3 is a diagram showing an example of an equilibrium state diagram for predicting the amount of liquid phase generated during sintering.
  • FIG. 4 is a photograph showing an example of a sample having a small difference in outer diameter shrinkage in the examples.
  • FIG. 5 is a photograph showing an example of a sample having a large outer diameter shrinkage difference in the examples.
  • the aluminum powder mixture according to the present embodiment 5% by mass or more and 30% by mass or less of the aluminum alloy powder made of the pure aluminum and the aluminum alloy having a lower melting point than the aluminum alloy is added to the starting powder made of pure aluminum or the aluminum alloy. It is a mixed aluminum powder mixture.
  • the aluminum alloy powder contains 1 or 2 types of Si and Cu in an amount of 5% by mass or more and 20% by mass or less, and Mg in an amount of 0.2% by mass or more and 2.0% by mass, and the balance is unavoidable impurities and aluminum. It consists of an aluminum alloy having a composition.
  • This aluminum alloy may contain Bi in an amount of 0.1% by mass or more and 1.0% by mass or less in addition to the above-mentioned contents of Si and Cu (1) or 2 and Mg.
  • the components of the aluminum alloy constituting the aluminum alloy powder of this embodiment will be described.
  • the content of one or two of Si and Cu is preferably 5% by mass or more and 20% by mass or less. If the content of one or two of Si and Cu is less than 5% by mass, a sufficient melting point lowering effect cannot be obtained for pure aluminum, and even if the temperature is raised to a predetermined temperature during sintering, the liquid phase is sufficiently formed. It does not occur and there is a risk that sufficient sinterability cannot be obtained.
  • the aluminum alloy constituting the aluminum alloy powder preferably contains Mg in an amount of 0.2% by mass or more and 2.0% by mass or less. If the Mg content is less than 0.2% by mass, the effect of destroying the oxide film on the surface of the pure aluminum powder or the surface of the aluminum alloy powder is not sufficient, and there is a possibility that sufficient sinterability of the starting powder cannot be obtained. When the Mg content exceeds 2.0% by mass, the effect of improving the sinterability is not seen with respect to the addition amount of Mg. On the other hand, excess Mg dissolves in aluminum due to the destruction of the oxide film.
  • the melting point of the aluminum alloy is lowered, so that the difference between the degreasing decomposition temperature and the melting point of the binder component contained when used for laminated molding becomes small.
  • the undecomposed residue of the binder component tends to remain on the surface of the starting powder and may be a factor of inhibiting sintering, so that sufficient sintering may not be obtained.
  • the aluminum alloy constituting the aluminum alloy powder preferably contains Bi in an amount of 0.1% by mass or more and 1.0% by mass or less. If the Bi content is less than 0.1% by mass, the destructive effect of the oxide film on the surface of the aluminum alloy powder is not sufficient, and the wettability of the resulting melt is not sufficient, so that the starting powder can be sufficiently sintered. There is a risk that it will not be obtained. If the Bi content exceeds 1.0% by mass, it is not expected to improve the action and effect with respect to the increase in the addition amount, which leads to high cost, which is not preferable.
  • the aluminum powder used as the starting material powder in the present embodiment and the aluminum alloy powder added to the starting material powder have a particle size distribution having a volume-based frequency cumulative 50% diameter (D50) of 12 ⁇ m or more and 50 ⁇ m or less. If the volume-based frequency cumulative 50% diameter (D50) of these powders is less than 12 ⁇ m, segregation of particles is likely to occur, the packing density is likely to decrease, the sintering shrinkage is uneven, and the sintering shrinkage is uneven. However, there is a risk that the desired shape cannot be maintained.
  • the volume reference frequency cumulative 50% diameter (D50) exceeds 50 ⁇ m, the contact area between the particles with respect to the particle volume becomes small, so that the progress rate of sintering slows down and a sufficient density as a sintered body can be obtained. It may not be possible.
  • the oxygen concentration contained in the above-mentioned aluminum alloy powder is 1.0% by mass or less.
  • the oxygen concentration is 1.0% by mass or less, even if an oxide film is formed on the powder surface, the oxide film is thinly formed on the powder surface. Therefore, the liquid phase at the time of sintering. Does not adversely affect the generation of. If the oxygen concentration exceeds 1.0% by mass, the oxide film becomes too thick, which may hinder the formation of a liquid phase during sintering.
  • the starting powder made of pure aluminum or an aluminum alloy contains 5% by mass or more and 30% by mass or less of the pure aluminum and an aluminum alloy powder having a melting point lower than that of the aluminum alloy. If the content of the low melting point aluminum alloy powder is less than 5% by mass, the amount of aluminum alloy powder for forming a liquid phase at the time of sintering is small, so that the amount of liquid phase generated is small and sintering may not be sufficient. ..
  • the starting powder may contain an aluminum alloy powder in addition to the pure aluminum powder.
  • the aluminum alloy powder contained in the starting powder preferably has a melting point of 650 ° C. or higher in order to obtain a melting point difference from the aluminum alloy powder having a low melting point.
  • the aluminum alloy powder as a starting material preferably contains Mg in an amount of 0.2% by mass or more and 2.0% by mass or less.
  • the aluminum alloy powder as a starting material preferably contains Bi in an amount of 0.1% by mass or more and 1.0% by mass or less in addition to Mg. The effectiveness of containing Mg and Bi is as described above in the case where the aluminum alloy powder contains Mg and Bi.
  • Manufacturing method of aluminum sintered body In order to produce an aluminum sintered body using the above-mentioned aluminum powder mixture, a method of using the above-mentioned aluminum powder mixture as a raw material powder and filling it in a mold having a predetermined shape, or a method of filling the raw material powder with a thermosetting resin, A method of selectively spraying and laminating a binder containing a thermoplastic resin or a photocurable resin can be used.
  • the pure aluminum powder for forming the aluminum powder mixture can be produced, for example, by a method such as a nitrogen gas atomizing method.
  • the aluminum alloy powder for forming the aluminum powder mixture can be produced, for example, by the nitrogen gas atomizing method.
  • the powder when the powder is laminated to obtain a shape, it can be realized by repeatedly laminating the raw material powder using a selective binder spray. By repeated laminating, the raw material powder is fixed so as to have a shape that matches the desired three-dimensional shape. After the raw material powder is fixed, unnecessary powder is removed or degreased as necessary to obtain, for example, the cube-shaped green body 1 shown in FIG. 1 (a).
  • the green body 1 is housed in the heating furnace 2 as shown in FIG. 1 (b), and the temperature is 580 to 650 ° C. in a vacuum atmosphere, a reducing atmosphere or an inert gas without pressurization. Heat to a certain temperature and sinter. By heating to a temperature in this range, a liquid phase is generated from the low melting point aluminum alloy powder that is added and mixed with the starting powder and contained in the range of 5 to 30% by mass so as to fill the gap between the starting powders. The liquid phase gets wet and spreads, and isotropic shrinkage can be obtained.
  • heating may be performed at a heating rate of 10 ° C./min or less in the temperature range of 500 ° C. or higher at which the liquid phase formation starts. desirable.
  • a heating step in two or more stages aimed at promoting solid-phase sintering by maintaining the temperature below the formation temperature of the liquid phase and stabilizing the gaps between the particles. May be carried out.
  • FIG. 2 shows that when the aluminum powder mixture 3 is a mixture of a starting material powder 4 made of pure aluminum powder and an aluminum alloy powder 5 having a lower melting point than the starting material powder 4, the aluminum powder mixture 3 is about 580 to 650 ° C. It is explanatory drawing for modeling and showing the state heated to the temperature. The melting point of pure aluminum is about 660 ° C.
  • the liquid phase 6 is generated from the aluminum alloy powder 5 having a low melting point, and the liquid phase 6 wets and spreads in the gaps between the starting powders 4 existing around the liquid phase 6.
  • the melting point of the pure aluminum powder 4 is about 660 ° C.
  • the entire pure aluminum powder 4 is not completely melted in the above temperature range, but it is an interface portion between the pure aluminum powders 4 and the liquid phase 6 is formed. Since a part of the wet and spread part is mutually melted and fused, when it is cooled after heating for a predetermined time, finally, as shown in FIG. 2 (c), a dense sintered body 7 in which the whole is almost melted and integrated is obtained. Obtainable.
  • the state in which the sintered body 7 is generated in the heating furnace 2 is shown in FIG. 1 (c).
  • the obtained sintered body 7 can be finished by processing with a cutting tool 8 or surface polishing to obtain a product sintered body 9.
  • the sintered body 7 or the product sintered body 9 was manufactured by sintering an aluminum powder mixture 3 in which a low melting point aluminum alloy powder was mixed with 5% by mass or more and 30% by mass or less of the starting material powder 4, the starting material powder was produced. It has a dense structure in which the liquid phase effectively fills the gaps between the four. Therefore, it is possible to obtain a well-shaped and high-density sintered body 7 or a product sintered body 9 that is close to the desired shape. For example, it is possible to obtain an aluminum sintered body 7 or a product sintered body 9 having a relative density of 85% or more and a thermal conductivity of 160 W / mK or more.
  • the melting point has dropped in an appropriate range with respect to pure aluminum.
  • the liquid phase 6 can be effectively generated in a desired amount.
  • the effect of destroying the oxide film on the surface of the starting powder can be sufficiently obtained, and the wet and spread liquid phase 6 strongly strengthens the starting powders 4. As a result of being able to join, good sinterability can be obtained. Further, when Bi is contained in the aluminum alloy powder 5 in the above range, the effect of destroying the oxide film on the surface of the starting powder can be obtained more effectively, and good sinterability can be obtained. .. For example, when a thick oxide film is formed on the outer surface of the starting powder 4, this oxide film inhibits the bonding due to the formation of the liquid phase of the starting powder 4 by the liquid phase, and inhibits good sinterability. There is a risk.
  • the liquid phase amount estimated from the equilibrium state diagram of the aluminum alloy constituting the aluminum alloy powder 5 to be applied and the liquid phase amount estimated from the content of the aluminum alloy powder 5 are 10 of the entire aluminum powder mixture. It is desirable to select a combination of composition and sintering conditions such that the composition is about 30%.
  • the vertical axis temperatures are 600 ° C., 620 ° C., and 640 in the interpretation from the equilibrium state diagram shown in FIG.
  • Auxiliary lines A, B, and C (chain lines in FIG. 3) are drawn at each position of ° C in parallel with the horizontal axis, and the horizontal axis is Al 89.7 Si 10 Mg 0.3 / (Al 100 + Al 89.7 Si 10 ).
  • Auxiliary lines D and E (chain lines in FIG. 3) are drawn in parallel with the vertical axis at positions of 10% by mass and 20% by mass of the ratio of the amount of aluminum alloy powder and the amount of pure aluminum having the above composition.
  • the liquid phase amount is about 22.9% when 640 ° C. is selected, and about 5.5 mass% when 620 ° C. is selected, which is 600 ° C. If you select, it will be about 0%.
  • the mass ratio of 20% is selected, the liquid phase amount is about 57.5%, when 620 ° C is selected, it is about 22.7 mass%, and when 600 ° C is selected, it is about 11.2%.
  • the amount of liquid phase produced can be estimated from the state diagram showing the relationship between the mass ratio and the temperature of the pure aluminum powder and the aluminum alloy powder having a specific composition. As described above, select a combination of composition and sintering conditions so that the liquid phase amount estimated from the estimated liquid phase amount and the content of the aluminum alloy powder is about 10 to 30% of the entire aluminum powder mixture. Is desirable.
  • the powder having a particle size distribution in the above range as the starting powder 4 and the aluminum alloy powder 5
  • segregation of particles can be eliminated, and as a result, a decrease in packing density is prevented and the sintering shrinkage is uniform. Properties can be ensured and uneven sintering shrinkage can be prevented. From the above, it is possible to obtain an aluminum sintered body having a high density, matching a desired shape, and exhibiting a well-shaped and high thermal conductivity.
  • the aluminum mixed powders of Examples 1 to 14 and Comparative Examples 1 to 6 are mixed.
  • Each of these aluminum mixed powders is tapped into a graphite mold having an internal dimension of ⁇ 20 mm ⁇ H20 mm and then heated at 580 to 650 ° C. for 120 minutes in a vacuum atmosphere, a reducing atmosphere or an inert gas atmosphere as shown in Table 2.
  • sintered bodies of Examples 1 to 14 and Comparative Examples 1 to 6 were obtained.
  • the physical property values (relative density, dimensions, thermal conductivity) of each obtained sintered body were measured. The measurement method of each physical property value is shown below.
  • Oxygen concentration The oxygen concentration of each of the powder 1 and the powder 2 constituting the aluminum powder mixture was measured by using the inert gas melting-infrared absorption method.
  • Thermal conductivity was measured by the laser flash method using the "Xe Flash Analyzer LFA467 HyperFlash” (trade name) manufactured by NETZSCH after processing the obtained sintered body into a disk shape of ⁇ 10 mm ⁇ t2 mm. did.
  • Melting point difference Using a differential scanning calorimeter (DSC), the melting point of the heat absorption peak generated by melting of the aluminum powder mixture during heating from room temperature to 700 ° C. in an argon gas atmosphere is defined as the melting point M1 (° C.) of the powder 1. The difference from the melting point M2 (° C.) of the powder 2 was calculated as the melting point difference M1-M2 (° C.).
  • DSC differential scanning calorimeter
  • Table 1 shows the composition and average particle size of powder 1, the composition and average particle size of powder 2, and the mass mixing ratio of powder 1 and powder 2.
  • Table 2 shows the sintering atmosphere, sintering temperature, sintered body density, thermal conductivity, and outer diameter shrinkage difference.
  • Examples 1 to 8 pure aluminum powder is used as powder 1, and as powder 2, one or two types of Si and Cu are 5% by mass or more and 20% by mass or less, and Mg is 0.2% by mass or more and 2.0.
  • an aluminum alloy powder obtained by adding at least one of Mg: 0.3 to 0.5% by mass and Bi: 0.1 to 0.2% by mass to aluminum was used as powder 1 and powder 2 was used. Is an example using the above-mentioned powder 2.
  • the average particle size of the powder 1 is 12 to 50 ⁇ m, and the average particle size of the powder 2 is 15 to 50 ⁇ m.
  • the sintered body density was 2.30 or more, the thermal conductivity was a value exceeding 140, and the outer diameter shrinkage rate was 2% or less. Therefore, if it is a sintered body using an aluminum powder mixture in which the above-mentioned powder 1 and the above-mentioned powder 2 have the above-mentioned mass mixing ratio, the desired shape having high density, excellent thermal conductivity, and not losing its shape can be obtained. A sintered body having a matching shape could be obtained.
  • Comparative Example 1 had a low Si content and a sufficient sintering promoting effect could not be obtained.
  • Comparative Example 2 the amount of Si and the amount of Cu were large, and the amount of the liquid phase was too large, resulting in a large difference in outer diameter shrinkage.
  • Comparative Example 3 is a sample in which the Mg content was too high, but the thermal conductivity was lowered due to the influence of the increase in the amount of Mg solidified in aluminum and the influence of the decrease in the density of the sintered body.
  • Comparative Example 4 is a sample in which the Mg content was too low, but the sintered body density decreased. In Comparative Example 5, since the amount of powder 2 added was smaller than that of powder 1, sufficient sintering did not occur. In Comparative Example 6, since the amount of powder 2 added was too large with respect to powder 1, a liquid phase was generated more than necessary during sintering, the difference in outer diameter shrinkage was large, and it was difficult to maintain the shape of the sample.
  • the composition of powder 1 and powder 2 is adjusted and sintered in an appropriate temperature range while adjusting the blending ratio of powder 1 + powder 2 and the average particle size to a specific range as in the above-mentioned example. It was found that an excellent sintered body can be obtained.
  • FIG. 4 shows a photograph of the appearance of Example 1. Further, a photograph of the appearance of Comparative Example 4 is shown in FIG.
  • the sample shown in FIG. 4 had a well-shaped cylindrical shape, and almost no change in diameter was observed from the upper part to the lower part.
  • the sample shown in FIG. 5 has a columnar shape on the upper side, the lower side has a bulging shape over the entire circumference, and as a result, the difference in outer diameter shrinkage becomes large. From these comparisons, it was considered necessary to control the amount of liquid phase in order to maintain the shape of the sintered body, and it was considered advantageous to manufacture the sintered body while densifying with the minimum liquid phase.
  • the aluminum powder mixture of the present invention sintering between powders (particles) can be further promoted, high density can be realized as an aluminum sintered body, and high electrical conductivity and high thermal conductivity are exhibited. Since it is possible to obtain a sintered body, it can be used industrially.

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EP4434653A1 (en) * 2023-03-22 2024-09-25 Ricoh Company, Ltd. Aluminum powder mixture, metal additive manufacturing powder, and additively manufactured metal product
WO2024195259A1 (ja) * 2023-03-22 2024-09-26 株式会社日立製作所 付加製造条件の決定装置、付加製造条件の決定方法、及び付加製造物の製造方法
JP7843011B1 (ja) * 2025-09-05 2026-04-09 三菱マテリアル株式会社 アルミニウム合金粉末焼結体

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WO2023063170A1 (ja) * 2021-10-14 2023-04-20 三菱マテリアル株式会社 アルミニウム粉末混合物、金属積層造形用粉末および金属積層造形物
JPWO2023181994A1 (https=) * 2022-03-24 2023-09-28

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EP4434653A1 (en) * 2023-03-22 2024-09-25 Ricoh Company, Ltd. Aluminum powder mixture, metal additive manufacturing powder, and additively manufactured metal product
WO2024195259A1 (ja) * 2023-03-22 2024-09-26 株式会社日立製作所 付加製造条件の決定装置、付加製造条件の決定方法、及び付加製造物の製造方法
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