WO2020021701A1 - 高速流体噴射装置 - Google Patents

高速流体噴射装置 Download PDF

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Publication number
WO2020021701A1
WO2020021701A1 PCT/JP2018/028223 JP2018028223W WO2020021701A1 WO 2020021701 A1 WO2020021701 A1 WO 2020021701A1 JP 2018028223 W JP2018028223 W JP 2018028223W WO 2020021701 A1 WO2020021701 A1 WO 2020021701A1
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WIPO (PCT)
Prior art keywords
gas
metal
melt
flow path
liquid film
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PCT/JP2018/028223
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English (en)
French (fr)
Japanese (ja)
Inventor
吉田健二
▲高▼橋亨
Original Assignee
株式会社東北マグネットインスティテュート
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 株式会社東北マグネットインスティテュート filed Critical 株式会社東北マグネットインスティテュート
Priority to CN201880062393.5A priority Critical patent/CN111182986B/zh
Priority to PCT/JP2018/028223 priority patent/WO2020021701A1/ja
Priority to JP2019500902A priority patent/JP6533352B1/ja
Publication of WO2020021701A1 publication Critical patent/WO2020021701A1/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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys

Definitions

  • the present invention relates to a unit for a metal powder manufacturing apparatus, a metal powder manufacturing apparatus, and a metal powder manufacturing method.
  • a unit for a metal powder manufacturing apparatus using a liquid film, a metal powder manufacturing apparatus, and a metal powder manufacturing method about is a unit for a metal powder manufacturing apparatus using a liquid film, a metal powder manufacturing apparatus, and a metal powder manufacturing method about.
  • Patent Documents 1 to 4 An atomizing method for producing a metal powder by injecting a liquid into a flow path of a molten metal and pulverizing and solidifying the molten metal is known (for example, Patent Documents 1 to 4).
  • An atomizing method using gas and water is known (for example, Patent Document 5, Non-Patent Documents 1 and 2).
  • Patent Literature 5 disclose an atomizing method using gas and water, but do not disclose a method for producing a desired metal powder with high yield.
  • the present invention has been made in view of the above problems, and has as its object to produce a desired metal powder with high yield.
  • the present invention is directed to a wall surrounding at least a part of a melt flow path in which a metal melt in which a metal is melted, a gas flow path provided in the wall and flowing a gas having a pressure higher than atmospheric pressure, and the gas flow path.
  • a chamber provided with an inner surface of the wall that communicates with the gas, and a gas injection hole that injects the gas in a direction in which the metal melt is accelerated, in the melt flow path, and a chamber downstream from a position where the gas is injected.
  • a liquid film forming section for forming a liquid film for solidifying the metal melt in the melt flow path.
  • the liquid film forming unit may include a liquid ejecting unit that ejects the liquid forming the liquid film toward the melt flow path.
  • the chamber may accelerate the metal melt in a direction in which the metal melt flows by injecting the gas into the metal melt
  • the liquid film forming unit may include the accelerated metal melt.
  • the liquid film may be formed such that the metal melt is solidified by contacting and / or approaching the liquid film with the body.
  • the gas flow path may be configured such that the interval gradually decreases toward the gas injection hole.
  • the gas injection holes may be provided to be substantially rotationally symmetric with respect to the center of the melt flow path.
  • a plurality of the gas injection holes may be arranged in a direction in which the metal melt flows.
  • a configuration may be adopted in which a heating unit that heats the gas before being injected is provided.
  • the liquid film forming unit may be configured not to form the liquid film at the center of the melt flow path but to surround the center and to form the liquid film to rotate around the center. it can.
  • the size of the cross section of the inner surface of the wall is in the direction in which the metal melt flows. It can be configured to gradually decrease as it goes and then gradually increase.
  • the present invention is a metal powder manufacturing apparatus including the above-described unit for a metal powder manufacturing apparatus and a supply unit for supplying the metal melt.
  • the present invention is provided on a wall surrounding at least a part of a melt flow path through which a metal melt in which metal is melted is provided on an inner surface of the wall in communication with a gas flow path through which a gas having a pressure higher than atmospheric pressure flows.
  • the gas is injected from a gas injection hole to the melt flow path in a direction to accelerate the metal melt, and the metal melt is solidified in the melt flow path downstream from a position where the gas is injected.
  • This is a method for producing a metal powder in which a liquid film to be formed is formed to form the metal powder.
  • a desired metal powder can be produced with high yield.
  • FIG. 1 is a sectional view of the metal powder manufacturing apparatus according to the first embodiment.
  • FIG. 2 is a sectional view of the atomizing unit according to the first embodiment.
  • FIG. 3 is a sectional view of an atomizing unit showing another example of the liquid film in the first embodiment.
  • 4A to 4E are cross-sectional views illustrating an example of a gas flow channel according to the first embodiment.
  • FIGS. 5A and 5B are cross-sectional views illustrating an example of a gas flow channel according to the first embodiment.
  • FIGS. 6A to 6C are plan views illustrating examples of the injection holes of the gas flow channel according to the first embodiment.
  • FIGS. 7A to 7C are cross-sectional views illustrating an example of a gas flow channel according to the first embodiment.
  • FIGS. 8A and 8B are cross-sectional views illustrating an example of the arrangement of the gas flow path and the liquid flow path in the first embodiment.
  • FIGS. 9A and 9B are cross-sectional views illustrating an example of the arrangement of the gas flow channel and the liquid flow channel in the first embodiment.
  • FIGS. 10A and 10B are plan views illustrating examples of the ejection holes of the liquid flow channel according to the first embodiment.
  • FIGS. 11A and 11B are plan views illustrating examples of the liquid flow channel according to the first embodiment.
  • FIG. 12 is a plan view illustrating an example of a liquid flow channel according to the first embodiment.
  • FIG. 13 is a cross-sectional view illustrating an example of a liquid flow channel according to the first embodiment.
  • FIG. 14A and 14B are cross-sectional views illustrating examples of the guide tube according to the first embodiment.
  • FIG. 15 is a cross-sectional view of an atomizing unit according to a first modification of the first embodiment.
  • FIG. 16 is a cross-sectional view of the metal powder manufacturing apparatus according to the example.
  • FIG. 17A is a diagram illustrating the X-ray diffraction spectra of Examples 1 to 6, and
  • FIG. 17B is a diagram illustrating the X-ray diffraction spectra of Comparative Examples 1 to 5.
  • FIG. 18A is a diagram illustrating the degree of amorphization with respect to the particle size D50 in the example and the comparative example, and
  • FIG. 18B is a diagram illustrating the particle size D50 with respect to the water pressure ratio.
  • a gas atomizing device and a liquid atomizing device are known.
  • a gas or a liquid is injected into or near a flow path of a metal melt.
  • the metal melt is cooled while applying a pulverizing force to the metal melt.
  • a metal powder so-called supercooled powder
  • the supercooled powder often has excellent corrosion resistance, wear resistance and / or magnetic properties.
  • the gas cooling ability is low, spherical droplets can be formed from the molten metal. Thereby, a spherical and small particle size metal powder can be obtained. However, it is difficult to cool the metal powder at a high cooling rate. Since the liquid atomizing device has a high liquid cooling capacity, the metal melt can be cooled at a high cooling rate.
  • Patent Document 2 describes that a rotational moment is given to an airflow sucked into an annular nozzle through which a molten metal flows, thereby turning the airflow in the annular nozzle. Since the metal melt is split by centrifugal force, it is possible to obtain a pseudo-spherical metal powder having a small particle size, a narrow particle size distribution width.
  • the yield of metal powder having a particle size of 5 ⁇ m or less is 50% or less. This is considered to be because the centrifugal force of the airflow is insufficient in crushing power.
  • the metal melt and the gas stream are in contact for a long time, the metal melt is cooled at a low speed. Therefore, an equilibrium phase is easily generated before the metal melt comes into contact with or close to the liquid, and it is difficult to produce a supercooled powder with high yield.
  • FIG. 1 is a sectional view of the metal powder manufacturing apparatus according to the first embodiment.
  • the metal powder manufacturing apparatus includes a supply unit 40, an atomizing unit 10 (a unit for a metal powder manufacturing apparatus), a recovery tank 50, and a guide tube 52.
  • An upward direction parallel to the central axis 60 is defined as a Z direction, and directions perpendicular to the central axis 60 are defined as an X direction and a Y direction.
  • the -Z direction is preferably the direction of gravity.
  • the supply unit 40 is a unit that melts a metal by heating it, and injects a metal melt to the atomizing unit 10 by applying pressure.
  • the injection direction of the metal melt is, for example, the ⁇ Z direction.
  • the atomizing unit 10 is a unit that generates a metal powder from a molten metal.
  • the atomizing unit 10 includes a chamber 11, a melt flow path 15, a gas flow path 20, and a liquid flow path 30.
  • the chamber 11 has an annular shape centered on the central axis 60 and is made of a metal such as an iron alloy.
  • a melt flow path 15 for transporting a metal melt is provided.
  • the gas passage 20 is provided in the wall of the chamber 11 and communicates with the injection hole 21.
  • the injection hole 21 is provided on the inner surface of the chamber 11 and injects gas into the melt flow path 15.
  • the liquid channel 30 is provided in the wall of the chamber 11 and communicates with the injection hole 31.
  • the injection hole 31 is provided on the inner surface of the chamber 11 and injects a liquid into the melt flow path 15. Details of the atomizing unit 10 will be described later.
  • the melt flow path 15 is a space surrounded by the wall of the chamber 11 and through which the metal melt flows.
  • the gas flow path 20 and the liquid flow path 30 are spaces provided in the wall of the chamber 11, and are filled with gas and liquid, respectively.
  • the injection holes 21 and 31 are holes in which the spaces of the gas flow path 20 and the liquid flow path 30 of the chamber 11 are exposed on the inner surface of the wall.
  • the material of the chamber 11 is made of, for example, iron, copper, nickel, aluminum or titanium, or an alloy thereof, and can be appropriately selected according to the process.
  • the atomizing unit 10 may be made of stainless steel.
  • the atomizing unit 10 may be made of a nickel alloy. If necessary, the metal surface may have a protective layer such as an oxide film.
  • the collection tank 50 collects the generated metal powder.
  • the liquid containing the metal powder is collected in the collection tank 50.
  • the guide tube 52 is provided along the liquid film 35, and the inner diameter gradually increases in the ⁇ Z direction.
  • the guide tube 52 protects the liquid film 35 from disturbance. For example, it is possible to prevent the metal powder or liquid splashed on the inner wall of the recovery tank 50 from affecting the liquid film 35.
  • FIG. 2 is a cross-sectional view of the atomizing unit according to the first embodiment.
  • the atomizing unit 10 is substantially circularly symmetric about the central axis 60.
  • the metal melt 45 passes through the melt flow path 15 in the chamber 11 in the ⁇ Z direction.
  • the metal melt 45 is a molten metal, for example, Fe (iron), Ni (nickel), Al (aluminum), Cu (copper), Co (cobalt), W (tungsten), Sn (tin), and / or It is a metal mainly composed of Ag (silver) or the like.
  • the chamber 11 has an upper chamber 12 and a lower chamber 13.
  • a gas flow path 20 is provided on a wall of the upper chamber 12, and an injection hole 21 is provided on an inner surface of the upper chamber 12.
  • a liquid flow path 30 is provided on a wall of the lower chamber 13, and an injection hole 31 is provided on an inner surface of the lower chamber 13.
  • the XY section of the upper chamber 12 is smaller than the XY section of the lower
  • the gas flow path 20 has a slit shape that is circularly symmetric about the central axis 60, and has a distal end portion 22 and a supply portion 23.
  • the gas having a pressure higher than the atmospheric pressure is introduced in the supply unit 23 in the horizontal direction toward the central axis 60.
  • the gas introduced into the supply unit 23 is pressurized above the atmospheric pressure by a gas compressor, a cylinder or a tank.
  • the gas pressure is, for example, 1.0 MPa.
  • the gas is, for example, air or an inert gas (for example, a rare gas such as nitrogen or argon).
  • the tip portion 22 is inclined in the ⁇ Z direction, and the interval between the slits gradually decreases toward the injection hole 21. Thereby, the injection speed of the gas 25 increases.
  • the injection hole 21 injects the gas 25 so as to include the ⁇ Z direction.
  • the metal melt 45 is accelerated by the gas 25.
  • the transport direction 45a of the metal melt 45 expands from the ⁇ Z direction. Since the diameter of the upper chamber 12 is small, the injection hole 21 can inject a gas near the metal melt 45. Thereby, the metal melt 45 can be further accelerated. Further, for example, the effect of adiabatic expansion of the gas from the injection holes 21 can be increased, and an additional cooling effect can be imparted to the gas.
  • the liquid flow path 30 has a slit shape, and has a tip portion 32 and a supply portion 33.
  • the liquid having a pressure higher than the atmospheric pressure is introduced horizontally in the supply unit 33 toward the central axis 60.
  • the liquid is a liquid for cooling the molten metal, for example, water.
  • Water used as a liquid may be, for example, an aqueous solution or ultrapure water, and a specific substance may be added to water or a specific substance may be removed. For example, oxygen or the like dissolved in water may be removed to prevent oxidation.
  • the pressure of the liquid is, for example, 60 MPa.
  • the tip 32 is inclined in the ⁇ Z direction, and the interval between the slits gradually decreases toward the injection hole 31.
  • the ejection holes 31 eject the liquid in the ⁇ Z direction.
  • the liquid film 35 is formed in the ⁇ Z direction.
  • the liquid film 35 has a single-lobed hyperboloidal shape as described in Patent Document 1, for example.
  • the liquid film 35 is not formed on the central axis 60, and the liquid film 35 rotates around the central axis 60.
  • the shape of the liquid film 35 is formed by a set of lines virtually extending in the direction in which the liquid is ejected, or a curved surface formed by the set of these lines, or This is because the shape is shifted in the ⁇ Z direction.
  • the metal melt 45 contacts or approaches the liquid film 35 in the region 51.
  • the metal melt 45 is pulverized by the liquid film 35 and cooled.
  • the metal melt 45 is rapidly cooled to generate metal powder.
  • the metal melt 45 may be pulverized by the gas 25 and cooled by the liquid film 35.
  • the wall of the chamber 11 surrounds at least a part of the melt flow path 15 through which the metal melt 45 in which the metal is melted flows.
  • the gas flow path 20 is provided on the wall of the chamber 11 and flows gas at a pressure higher than the atmospheric pressure.
  • the injection hole 21 (gas injection hole) is provided on the inner surface of the wall communicating with the gas flow path 20, and injects the gas 25 into the melt flow path 15 in a direction to accelerate the metal melt 45.
  • the injection hole 31 serving as a liquid film forming section forms a liquid film 35 that pulverizes and solidifies the metal melt 45 in the melt flow path 15 downstream from the position where the gas is injected.
  • the chamber 11 accelerates the metal melt 45 in the ⁇ Z direction (the direction in which the metal melt flows) by injecting the gas into the metal melt 45.
  • the injection holes 31 form the liquid film 35 such that the accelerated metal melt 45 contacts and / or approaches the liquid film 35 to solidify the metal melt 45.
  • the metal melt 45 can be pulverized.
  • a crushing force such as a shearing force is applied to the metal melt 45.
  • the metal melt 45 can be cooled by the gas 25 and the liquid film 35. Further, since the metal melt 45 is accelerated by the gas 25, the time from the cooling of the metal melt 45 by the gas 25 to the cooling of the metal melt 45 by the liquid film 35 can be reduced. Therefore, the cooling rate of the metal melt 45 can be increased. Therefore, a supercooled powder containing a large amount of a non-equilibrium phase or a supersaturated solid solution phase can be obtained.
  • the particle size of the metal powder can be adjusted by the balance between the gas pressure and the liquid pressure. Thereby, a supercooled powder having a desired particle size can be produced with a high yield. Thus, a desired metal powder can be produced with a high yield.
  • the pressure of the gas 25 injected from the injection hole 21 is preferably 0.15 MPa (1.5 atm) or more, more preferably 0.20 MPa (2.0 atm) or more. .50 MPa (5.0 atm) or more is more preferable.
  • the upper limit of the gas pressure is not particularly limited.
  • the pressure of the gas may be 5.0 MPa (50 atm) or less.
  • the pressure of the liquid ejected from the ejection hole 31 (that is, the pressure in the liquid flow path 30) is preferably 0.3 MPa (3.0 atm) or more, more preferably 6.0 MPa (60 atm) or more, and 50 MPa (500 atm). Or more).
  • the upper limit of the liquid pressure is not particularly limited, but may be, for example, 150 MPa (1500 atm) or less.
  • the injection hole 31 does not form the liquid film 35 at the center of the melt flow path 15 but forms the liquid film 35 so as to surround the center and rotate around the center. Since the liquid film 35 is not formed at the center of the melt flow path 15, the gas can move at high speed in the ⁇ Z direction through the center of the melt flow path 15. Thereby, the metal melt 45 is further accelerated, and the cooling rate of the metal melt 45 can be further increased. Since the liquid film 35 is rotating, the gas rotates at high speed in the region 51 of the liquid film 35. Due to this rotational force, the metal melt 45 is pulverized smaller.
  • the velocity of the gas around the metal melt 45 in at least a part of the melt flow path 15 is preferably supersonic.
  • the metal melt 45 can be pulverized by a supersonic shock wave.
  • the cooling rate of the metal melt 45 can be increased.
  • the velocity of the gas in the region 51 is supersonic.
  • the distance between the injection hole 21 and the region 51 be short in order to shorten the time required for rapid cooling (that is, landing) of the metal melt 45.
  • FIG. 3 is a sectional view of an atomizing unit showing another example of the liquid film in the first embodiment.
  • the liquid flow path 30 has a liquid film 35 in a cone shape, a conical shape, or an inverted cone shape as described in Patent Documents 3 and 4.
  • the vertex of the cone shape of the liquid film 35 is located, for example, on the central axis 60. Since the liquid film 35 is formed at the center of the melt flow path 15, the metal melt 45 contacts the liquid film 35 more. Thereby, the metal melt 45 can be cooled. Further, the metal melt 45 can be pulverized simultaneously with the cooling (secondary pulverization).
  • the shape of the liquid film 35 can be set arbitrarily. In order to pulverize the metal melt 45 smaller, it is preferable that the liquid film 35 has a single-lobed hyperboloidal shape centered on the central axis 60.
  • FIGS. 4A to 5B are cross-sectional views illustrating an example of a gas flow path according to the first embodiment.
  • the gap between the slits of the distal end portion 22 of the gas flow path 20 gradually decreases toward the injection hole 21.
  • the gap between the slits of the distal end portion 22 of the gas flow path 20 gradually increases toward the injection hole 21.
  • the tip end portion 22 of the gas flow path 20 has a substantially uniform interval between slits.
  • the distal end portion 22 of the gas flow path 20 gradually increases after the gap between the slits gradually decreases toward the injection hole 21.
  • the tip 22 has a shape like a Laval nozzle, for example.
  • a spiral groove 24 may be formed on the inner surface of the tube.
  • the supply unit 23 and the distal end portion 22 are curved in the ⁇ Z direction along the central axis 60 in the XZ plane (or the YZ plane).
  • the supply portion 23 and the tip portion 22 extend linearly in the ⁇ Z direction along the central axis 60 in the XZ plane (or the YZ plane).
  • the gas flow path 20 may have a supply section 23 extending in the XY plane and a tip section 22 inclined in the ⁇ Z direction.
  • the supply section 23 of the gas flow path 20 may be inclined in the ⁇ Z direction.
  • the shape of the distal end portion 22 of the gas flow path 20 can be appropriately designed. As shown in FIG. 4A, it is preferable that the interval of the tip end portion 22 of the gas flow path 20 gradually decreases toward the injection hole 21. Thereby, the injection speed of the gas from the injection holes 21 can be increased. Further, as shown in FIG. 4D, it is preferable that the interval of the tip end portion 22 gradually decreases toward the injection hole 21 and then gradually increases. Thereby, the injection speed of the gas from the injection holes 21 can be increased. From the viewpoint of accelerating the metal melt 45, the apex angle ⁇ of the gas 25 (see FIG. 3) is preferably, for example, 0 ° to 100 °.
  • FIG. 6 (a) to 6 (c) are plan views showing examples of gas injection holes in the first embodiment.
  • 6A to 6C show the XY plane shapes of the injection holes 21.
  • FIG. 6A the injection hole 21 is a ring-shaped slit having an annular shape centered on the central axis 60.
  • FIG. 6 (b) it is a perforated pencil type in which a plurality of injection holes 21 are provided along a circle 61 centered on a central axis 60.
  • FIG. 6C the injection holes 21 are provided only on the ⁇ X side with respect to the central axis 60.
  • the shape of the injection hole 21 can be appropriately designed. As shown in FIGS. 6A and 6B, it is preferable that the injection holes 21 be provided substantially rotationally symmetric with respect to the center of the melt flow path 15 so as to have a manufacturing error. As a result, the gas 25 is uniformly injected to the metal melt 45. Therefore, the metal melt 45 can be accelerated efficiently.
  • the width of the injection hole 21 is, for example, 0.1 mm to 5 mm.
  • the injection hole 21 may have a structure that opens when gas pressure is applied.
  • the entire area of the injection hole 21 is, for example, 0.5 mm 2 to 1000 mm 2 .
  • FIGS. 7A to 7C are cross-sectional views illustrating an example of a gas flow path according to the first embodiment.
  • a plurality of gas channels 20a to 20c are provided in the Z direction.
  • the injection holes 21a to 21c are arranged in the upper chamber 12 in the Z direction.
  • the shapes of the gas flow paths 20a to 20c may be the same or different.
  • the injection holes 21a to 21c may have the same shape or different shapes.
  • a plurality of tips 22a and 22b branch from one supply unit 23.
  • a plurality of injection holes 21a and 21b are arranged on the inner surface of the upper chamber 12 in the Z direction.
  • the injection holes 21a and 21b may have the same shape or different shapes.
  • a plurality of injection holes 21a to 21c are arranged in the Z direction. Thereby, the metal melt 45 can be further accelerated.
  • the atomizing unit 10 includes a heating unit 26 (for example, a heater) for heating the gas.
  • the heating section 26 heats the gas in the gas flow path 20. This causes the gas to be above room temperature.
  • the gas velocity is increased.
  • the gas is heated.
  • the temperature of the gas is preferably, for example, 100 ° C. or higher.
  • FIGS. 8A to 9B are cross-sectional views illustrating examples of the arrangement of the gas flow channel and the liquid flow channel in the first embodiment.
  • an upper chamber 12 having a gas flow path 20 and a lower chamber 13 having a liquid flow path 30 are separated.
  • the atomizing unit 10 may be divided into a plurality.
  • the central axis 60a of the upper chamber 12 does not coincide with the central axis 60b of the lower chamber 13.
  • the central axes 60a and 60b do not need to coincide with each other, but it is preferable that the central axes 60a and 60b coincide with each other in order to uniformly pulverize the metal melt 45.
  • the injection holes 21 of the gas flow path 20 are provided in the ⁇ Z direction from the injection holes 31 of the liquid flow path 30.
  • the injection hole 21 may be located downstream of the injection hole 31.
  • the injection holes 21 are preferably arranged in the + Z direction from the region 51 in order to primary crush the metal melt 45 before the metal melt 45 contacts or approaches the liquid film 35.
  • the chamber 11 has a constricted portion 14 between the position where the injection hole 21 injects the gas and the position where the metal melt 45 contacts or approaches the liquid film 35.
  • the size of the XY cross section of the inner surface of the wall of the chamber 11 gradually decreases as going in the ⁇ Z direction, and then gradually increases.
  • the constriction 14 has, for example, a Laval nozzle shape.
  • the constricted portion 14 functions as a Laval nozzle, and makes the gas passing through the constricted portion 14 high speed (for example, supersonic speed). Thereby, the cooling rate of the metal melt 45 can be increased.
  • the injection hole 31 may be provided in the constriction portion 14.
  • the injection hole 31 may be provided at a point where the XY cross section of the inner surface of the wall of the chamber 11 becomes minimum.
  • FIGS. 10A and 10B are plan views illustrating examples of the ejection holes of the liquid flow channel according to the first embodiment.
  • FIGS. 10A and 10B show the XY plane shapes of the injection holes 31.
  • FIG. 10A the injection hole 31 is annular with the center axis 60 as the center.
  • FIG. 10B a plurality of injection holes 31 are provided along a circle 61 centered on a central axis 60.
  • the shape of the injection hole 31 can be appropriately designed.
  • the injection holes 31 be provided substantially rotationally symmetric about the central axis 60 to the extent of a manufacturing error. For example, as shown in FIG.
  • the distance between the center axis 60 and a straight line extending from the injection hole 31 in the direction of the central axis 60 to the center line of the tip 32 is Even when the minimum position in the Z direction is + Z side from the position in the Z direction where the distance between the center axis 60 and the straight line extending from the injection hole 21 in the direction of the center axis 60 to the center line of the distal end portion 22 is minimum. It may be on the ⁇ Z side. Further, for example, as shown in FIG.
  • the XZ section (or the YZ section) including the center axis 60 has The intersection of the straight line extending from the injection hole 31 to the central axis 60 and the central axis 60 (the apex of the plane (cone) formed by the center line of the distal end portion 32) is defined by the central axis of the distal end portion 22 and the central axis. It may be on the + Z side or on the -Z side of the intersection (the vertex of the plane (cone) formed by the center line of the distal end portion 22) between the straight line extended to 60 and the central axis 60.
  • FIGS. 11A, 11B, and 12 are plan views illustrating examples of the liquid flow channel according to the first embodiment.
  • an injection hole 31 is provided on the inner surface of the lower chamber 13.
  • a distal end portion 32 is provided so as to surround the injection hole 31.
  • a supply section 33 is provided so as to surround the tip section 32.
  • the tip portion 32 is provided with a revolving wing 34.
  • the swirling blade 34 applies a counterclockwise rotational moment to the liquid 39b introduced from the supply unit 33.
  • the liquid 39 a having a rotational moment is injected from the injection hole 21 to the melt flow path 15. Thereby, the liquid film 35 formed by the liquid 39a rotates, and becomes, for example, a single-leaf hyperboloid.
  • the swirl wings 34 are shorter and thicker than those in FIG. 11 (a).
  • the swirling blade 34 applies a clockwise rotation moment to the liquid 39a introduced from the supply unit 33.
  • the swirl vanes 34 are not provided in the liquid flow path 30.
  • the introduction pipe 36 introduces the liquid 39c into the supply unit 33 with offset.
  • the introduction pipe 36 introduces the liquid 39c in a tangential direction of a circle centered on the central axis 60, for example.
  • the liquid 39 a to which the rotational moment has been applied is ejected from the ejection hole 31.
  • Other configurations are the same as those in FIG.
  • the swirling portion can be appropriately set so as to impart a rotational moment to the liquid film 35.
  • the liquid film 35 does not have a rotational moment, the liquid film 35 having a cone shape as shown in FIG. 3 can be formed.
  • the ejection direction of the liquid 39a ejected from the ejection holes 31 to the melt flow path 15 is a component in a circumferential direction of a circle centered on the central axis 60 in the XY plane. Directions.
  • the ejection direction of the liquid 39a ejected from the ejection hole 31 to the melt flow path 15 is a circumferential component of a circle centered on the central axis 60 on the XY plane and a direction component toward the central axis 60 (radial component). ) May be included.
  • Such a jet direction of the liquid 39a can be formed by, for example, the wall surface of the revolving wing 34 or the wall surface (inner surface) of the introduction pipe 36 in FIG. 11A or 11B.
  • the liquid film forming unit includes an injection hole 31 (liquid injection unit) for injecting the liquid forming the liquid film 35 toward the melt flow path 15. Thereby, the liquid film 35 can be easily formed.
  • FIG. 13 is a cross-sectional view illustrating an example of the liquid flow path according to the first embodiment.
  • a plurality of liquid flow paths 30a to 30c are provided on the wall of the lower chamber 13 in the Z direction.
  • the injection holes 31a to 31c are arranged in the Z direction on the inner surface of the lower chamber 13.
  • the shapes of the liquid channels 30a to 30c may be the same as each other, or may be different from each other.
  • the injection holes 31a to 31c may have the same shape or different shapes.
  • a plurality of injection holes 31a to 31c may be arranged in the Z direction. Thereby, a plurality of liquid films 35 can be formed. Since the metal melt 45 contacts or approaches the plurality of liquid films 35, the metal powder can be pulverized smaller. Further, the cooling rate of the metal melt 45 can be increased.
  • the temperature of the liquid ejected from the ejection holes 31 is preferably lower than room temperature.
  • the temperature of the liquid film 35 may be higher than room temperature.
  • FIGS. 14A and 14B are cross-sectional views illustrating examples of the guide tube according to the first embodiment.
  • an introduction pipe 53 for introducing a liquid 54 from outside to inside of the guide pipe 52 is provided.
  • the liquid 54 is a coolant such as water, for example, and cools the inside of the guide tube 52.
  • the cooling rate of the metal melt 45 decreases.
  • the inner diameter of the inner surface of the guide tube 52 gradually decreases in the ⁇ Z direction, and then gradually increases.
  • the inner surface of the guide tube 52 has a Laval nozzle shape. Thereby, the gas in the guide tube 52 is accelerated in the ⁇ Z direction. Thereby, the speed of the metal melt 45 can be increased. Therefore, the cooling rate of the metal melt 45 can be increased.
  • the shape of the guide tube 52 can be appropriately set so as to protect the liquid film 35.
  • the guide tube 52 is preferably provided along the liquid film 35 from the viewpoint of protecting the liquid film 35.
  • a spiral groove may be provided on the inner surface of the guide tube 52.
  • FIG. 15 is a cross-sectional view of an atomizing unit according to a first modification of the first embodiment.
  • the atomizing unit 10 includes an upper chamber 12 having a gas flow path 20 and a rotating body 37.
  • the inner surface of the rotator 37 has, for example, a one-lobe hyperboloid shape, and rotates about a central axis 60.
  • the introduction pipe 38 introduces the liquid 39 d into the inner surface of the rotating body 37.
  • the rotating liquid film 35 is formed on the inner surface of the rotating body 37.
  • the liquid film 35 may be formed by the rotating body 37.
  • the liquid film forming section may form the liquid film 35 that solidifies the metal melt 45.
  • the metal melt 45 can be pulverized (secondary pulverization).
  • the unit for a metal powder manufacturing apparatus includes a wall surrounding at least a part of the melt flow path 15 through which the metal melt 45 in which the metal is melted, and a gas provided at the wall and having a pressure higher than the atmospheric pressure.
  • a gas flow path 20 that flows, a gas injection hole 21 that is provided on an inner surface of a wall that communicates with the gas flow path 20, and that injects gas into the melt flow path 15 in a direction in which the metal melt 45 is accelerated;
  • the liquid ejecting unit of the unit for a metal powder manufacturing apparatus can form a liquid film 35 for solidifying the metal melt 45 in the melt flow path 15 downstream from the position where the gas is ejected.
  • the unit for a metal powder manufacturing apparatus includes a wall surrounding at least a part of the melt flow path 15 through which the metal melt 45 in which the metal is melted, and a wall provided on the wall and higher than the atmospheric pressure.
  • a gas flow path 20 through which a gas having a pressure flows; and a gas injection hole 21 provided on an inner surface of a wall communicating with the gas flow path 20 and injecting gas into the melt flow path 15 in a direction to accelerate the metal melt 45.
  • a rotating body 37 whose wall is rotatable around a central axis 60 of the melt flow path 15.
  • the metal flow is supplied to the melt flow path downstream from the position where the gas is injected.
  • a liquid film 35 that solidifies the body 45 can be formed.
  • the above-described unit for a metal powder manufacturing apparatus includes a wall surrounding at least a part of the melt flow path 15 through which the metal melt 45 in which the metal is melted, and a gas provided on the wall and having a pressure higher than the atmospheric pressure.
  • a flowing gas flow path 20 and a gas injection hole 21 which is provided on the inner surface of the wall in communication with the gas flow path 20 and injects gas into the melt flow path 15 in a direction in which the metal melt 45 is accelerated.
  • a liquid film forming section for forming a liquid film 35 for solidifying the metal melt 45 in the melt flow path 15 downstream from the position where the gas is injected.
  • the upper limit of the particle size D50 at a cumulative frequency of 50% of the metal powder is preferably less than 20 ⁇ m, more preferably 10 ⁇ m or less, and even more preferably 8.0 ⁇ m or less.
  • the lower limit of the particle size D50 at which the cumulative frequency of the metal powder is 50% is not particularly limited.
  • the lower limit of the particle size D50 may be 0.02 ⁇ m from the viewpoint of the accuracy of the microtrack described later.
  • the lower limit of the particle size D50 may be 0.50 ⁇ m, 1.0 ⁇ m, or 2.0 ⁇ m.
  • the lower limit of the degree of amorphization is preferably 80% or more, more preferably 90% or more, and even more preferably 95% or more.
  • the upper limit of the degree of amorphization is 100%.
  • the upper limit of the particle size D50 at which the cumulative frequency of the metal powder is 50% is preferably 100 ⁇ m or less, more preferably 80 ⁇ m or less, and even more preferably 50 ⁇ m or less.
  • the lower limit of the particle size D50 of the 50% cumulative frequency of the metal powder is preferably 20 ⁇ m or more.
  • the lower limit of the degree of amorphization is preferably 60% or more, more preferably 70% or more, and even more preferably 80% or more.
  • the upper limit of the degree of amorphization is 100%.
  • the numerical conditions relating to the above effects are not particularly limited.
  • an amorphous state is obtained in an iron alloy in which the amount of Fe is 80 atomic% or more, it is particularly preferable that the above-described effect is obtained.
  • FIG. 16 is a cross-sectional view of the metal powder manufacturing apparatus according to the example.
  • the supply unit 40 has a heating tank 42, a heating unit 44, and an ejection hole 46.
  • the master alloy 48 is introduced into the heating tank 42.
  • the heating unit 44 induction-heats and melts the mother alloy 48 in the heating tank 42.
  • the molten metal is ejected from the ejection holes 46.
  • the atomizing unit 10 includes a chamber 11, a melt flow path 15, a gas flow path 20, and a liquid flow path 30.
  • the diameter of the inner surface of the upper chamber 12 is smaller than the diameter of the inner surface of the lower chamber 13 and gradually decreases in the ⁇ Z direction.
  • the injection hole 21 is provided at the ⁇ Z end of the upper chamber 12.
  • the diameter of the inner surface of the lower chamber 13 gradually decreases after gradually decreasing in the ⁇ Z direction.
  • a swirl vane 34 is provided at the tip 32 of the liquid channel 30.
  • An injection hole 31 is provided near the smallest diameter of the inner surface of the lower chamber 13.
  • the liquid film 35 that rotates around the central axis 60 is formed by the liquid ejected from the ejection holes 31.
  • a guide tube 52 is provided to protect the liquid film 35.
  • Other configurations are the same as those in FIGS. 1 and 2 of the first embodiment, and a description thereof will be omitted.
  • Metal powder was produced using the metal powder manufacturing apparatus of the example. Fe, Fe—Si, Fe—B, Fe—P, and Cu were adjusted to have a composition (atomic weight composition) of Fe 83.3 Si 4 B 8 P 4 Cu 0.7 .
  • a molten mother alloy 48 having a desired composition was produced.
  • the mother alloy 48 was crushed and filled in the heating tank 42.
  • the heating unit 44 induction-heats the mother alloy 48 in an argon atmosphere to 1350 ° C.
  • the metal melt 45 supplied from the supply unit 40 was pulverized by the atomizing unit 10 and cooled and solidified to obtain a metal powder.
  • As the gas flowing through the gas flow path 20 air at 20 ° C. in atmospheric pressure was used, and as the liquid flowing in the liquid flow path 30, water at 25 ° C. in atmospheric pressure was used. Contaminants and condensed particles were removed from the metal powder through a vibrating sieve.
  • Table 1 is a table showing the production conditions of the metal powders of Examples 1 to 6 and Comparative Examples 1 to 5, and the measurement results of the structural phase and the particle size.
  • the “gas pressure ratio” is a value obtained by standardizing the pressure of the gas in the gas flow path 20 with the gas pressure of the first embodiment.
  • the “gas flow rate ratio” is a value obtained by standardizing the gas flow rate in the injection hole 21 with the gas flow rate in the first embodiment.
  • the “water pressure ratio” is a value obtained by normalizing the pressure of water in the liquid flow path 30 with the water pressure of the first embodiment.
  • “Swirl wing” indicates the presence or absence of the swirl wing 34. When there are swirling wings, the liquid film 35 has a one-leaf hyperboloid, and when there is no swirling wing, the liquid film 35 has a cone shape.
  • Phase is a phase identified by an X-ray diffraction (XRD) method, where Amo indicates an amorphous phase and Cry indicates a crystalline phase.
  • Amorphization degree indicates the ratio of amorphous obtained by the X-ray diffraction method.
  • D50 is the particle size D50.
  • Example 1 to 6 gas was injected from the injection hole 21 and gas was forcibly introduced into the melt flow path 15.
  • the liquid film 35 was formed into a single-leaf hyperboloid, and the water pressure ratio was changed.
  • Example 4 to 6 the liquid film 35 was formed in a cone shape, and the water pressure ratio was changed.
  • Comparative Examples 1 to 5 no gas is injected from the injection holes 21 and the gas in the melt flow path 15 is air that naturally flows in from above.
  • the liquid film 35 was formed in a cone shape, and the water pressure ratio was changed.
  • the liquid film 35 was formed into a single-leaf hyperboloid, and the water pressure ratio was changed.
  • FIG. 17A is a diagram showing X-ray diffraction spectra of Examples 1 to 6, and FIG. 17B is a diagram showing X-ray diffraction spectra of Comparative Examples 1 to 5.
  • FIG. 17A in Examples 1 to 4, no peak due to the crystal phase is observed. In Example 5, a small peak is observed. In Example 6, a rather large peak is observed.
  • Table 1 in Examples 1 to 3 and 6, the structural phase is an amorphous phase and the degree of non-crystallinity is 100%. It can be seen that the structural phases of Examples 4 and 5 are an amorphous phase and a crystalline phase. In Examples 4 and 5, the degree of amorphization is slightly reduced to 72% and 97%.
  • FIG. 18A is a diagram showing the degree of amorphization with respect to the particle size D50 in Examples and Comparative Examples
  • FIG. 18B is a diagram showing the particle size D50 with respect to the water pressure ratio.
  • the numbers indicate Examples 1 to 6 and Comparative Examples 1 to 5.
  • the degree of amorphization is as small as 50% or less.
  • the particle size D50 is small and the degree of amorphization is 100%.
  • the degree of amorphization is higher than that of Comparative Example.
  • the degree of amorphization can be increased as compared with the comparative example.
  • the particle size D50 can be smaller and the degree of non-crystallization can be larger than in Examples 4 to 6 in which the liquid film 35 has a cone shape.
  • the particle size of the metal powder can be controlled by changing the water pressure.
  • the degree of amorphization of the metal powder can be increased as compared with the comparative example. This is because the gas flow path 20 injects gas from the injection holes 21 to the metal melt 45, thereby accelerating the metal melt 45. When the metal melt 45 is accelerated, the metal melt 45 contacts or approaches the liquid film 35 at a high temperature. Thereby, the metal melt 45 is rapidly cooled at the same time as the pulverization or immediately after (almost simultaneously). Therefore, the metal powder is formed in an amorphous state. As described above, in the example, a metal powder containing a large amount of supercooled structure such as a non-equilibrium phase or a supersaturated solid solution phase can be produced with high yield. Further, by controlling the ratio between the water pressure and the gas pressure, the particle size of the metal powder can be controlled.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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CN112589109B (zh) * 2020-11-27 2022-03-25 佛山市中研非晶科技股份有限公司 气雾化制粉方法及应用其的气雾化制粉系统
CN113102762A (zh) * 2021-04-09 2021-07-13 上海大学 一种金属粉末的制备方法及装置
CN114713828A (zh) * 2022-03-11 2022-07-08 北京七弟科技有限公司 Mim用钛及钛合金球形或近球形金属粉末的制备方法

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