JP5388272B2 - Metal particle manufacturing method - Google Patents

Description

The present invention relates to a method for producing metal particles by melting and dropping a metal material obtained by twisting two kinds of wires made of metals having different melting points while rotating .

  A conventional technique for producing metal particles is a rotating electrode method. In this method, a rotated columnar metal material electrode is melted by arc discharge and scattered to produce metal particles.

  Another conventional technique for producing metal particles is a melt dropping method. In this method, metal particles melted in a crucible are dropped from a nozzle to produce metal particles.

  Another conventional technique for producing metal particles is a forming granulation method. This method produces metal particles by compression molding of a mold.

  Another conventional technique for producing metal particles is a melting method by induction heating. In this method, metal particles are gradually melted in one direction by an induction heating coil to produce metal particles.

  Patent Document 1 describes a titanium-aluminum intermetallic compound powder forming method in which a composite wire is supplied, melted with a laser beam, an inert gas is injected to form a powder, and an intermetallic compound is solidified. ing.

  In Patent Document 2, a laser beam is converged by a parabolic mirror, a wire is fed from a hole provided in the mirror toward the focal point of the laser beam, and a gas is flowed coaxially with the wire and melted by the laser beam. An apparatus for producing fine powder by a laser that atomizes the melted portion of the wire by blowing the tip portion of the wire with the gas is described.

  Patent Document 3 describes a method for producing a fine powder using a laser beam.

  In Patent Document 4, two or more kinds of fine metal wires having a diameter of 5 mm or less are bundled in a weight ratio of a target composition and integrated into a composite rod having a diameter of 10 mm or more, and the composite rod is a shaft thereof in an inert gas atmosphere. While rotating at 1000 rpm or more around the center, one end of the composite rod is heated and melted by irradiation with an electron beam, or melted by arc heat between the electrodes facing the one end and scattered as particles. A process for producing an intermetallic compound powder characterized in that it is made to be described.

Japanese Patent Laid-Open No. 10-1767 JP-A-62-177107 JP-A-3-13510 JP-A-1-222002

  Metal particles that are used as neutron multiplication materials in fusion reactor blankets or lightweight heat-resistant materials for aviation, space, automobiles, etc. are metal particles that do not contain impurities, and the produced metal particles are intermetallic compounds or In some cases, metal particles that are formed of an alloy and have a uniform structure due to a small thermal shock during production may be required. Moreover, in the production of these metal particles, it is required that the initial metal material can be easily adjusted and is mass-productive.

  In the production of metal particles by the conventional rotating electrode method, a rod-shaped electrode is required, and when an intermetallic compound is used for this electrode, there is a problem that it is difficult to manufacture the electrode. Moreover, since it melts by arc discharge, there exists a problem that a thermal shock is large. In the production of metal particles by the conventional melt dropping method, the metal melted in the crucible is dripped from the nozzle. Therefore, when producing a material such as an intermetallic compound having a high melting point, impurities are caused by reaction with the crucible material. It will be mixed.

  In the production of metal particles by the conventional forming granulation method, it is necessary to produce an alloy powder as a starting metal material, and there is a problem in the uniformity of the produced metal particles.

  In the conventional method of producing metal particles by the induction heating melting method, there is an advantage that impurities are not mixed because it is non-contact as an advantage of the floating zone melting method, but it is difficult to attach a temperature gradient and heating. It was difficult to adjust the heating because the part was wide and it was difficult to produce a uniform intermetallic compound or alloy.

  Furthermore, in the manufacturing apparatus shown in Patent Document 1, a laser beam is used, but since a fine powder is manufactured, a powder is formed by injecting an inert gas to form a uniform powder. It is difficult to produce metal particles having a structured structure.

  In view of this point, the present invention has no melting of impurities, no thermal shock during production, and ensures a sufficient melting temperature and melting time to obtain a uniform structure, for example, an intermetallic compound or alloy having a uniform structure. An object of the present invention is to provide a metal particle production apparatus and a metal particle production method that can be easily adjusted for the starting metal material and are suitable for mass production.

The present invention relates to a metal particle production apparatus including a sealed container and a heating device that heats and melts a wire or an elongated rod-shaped metal material supplied to the sealed container.
A metal material supply device that supplies the sealed container while rotating the metal material,
The sealed container is in a vacuum state or an inert gas atmosphere,
Having a light source disposed inside or outside the sealed container, forming a light heating portion that performs light heating by concentrating on the metal material with light from the light source, melting the metal material by light heating, The molten metal is rotated and held at an adjacent molten metal holding portion to homogenize the molten metal, and is kept non-contacted until it drops to a size that drops as metal particles by gravity. Provided is a metal particle production apparatus comprising a light heating melt dripping means for forming a molten particulate material.

  The present invention also provides a metal particle manufacturing apparatus, wherein the light heating melt dripping means includes a heating control means for controlling a melting temperature of the metal material.

  The present invention also provides the metal particle manufacturing apparatus, wherein the heating and melting dripping means includes a lamp and a condensing mirror for condensing light emitted from the lamp, or a laser light source. To do.

  The present invention also includes a metal particle cooling unit that cools the dropped metal particles during the dropping, and a metal particle collecting unit connected to the metal particle cooling unit, and the metal particle cooling unit is inclined inside. An apparatus for producing metal particles is provided that has an inclined portion that collides with falling metal particles.

The present invention, in a metal particle production method by a metal particle production apparatus comprising a sealed container and a heating device for heating and melting and dropping a wire or elongated rod-shaped metal material supplied to the sealed container,
A metal material supply device supplies a metal material to the sealed container, the inside of the sealed container is in a vacuum state or an inert gas atmosphere, and the metal is irradiated with light from a light source disposed inside or outside the sealed container. Light heating that heats the material in a non-contact manner, melts and drops in a particulate form, and heats the light by concentrating on the metal material by light heating using the light heating melt dripping means. Form the part, melt the metal material by light heating, rotate and hold the molten metal at the adjacent molten metal holding part where light heating is not concentrated and homogenize the molten metal, the molten metal is non-contact Thus, the method for producing metal particles is characterized in that the holding is continued until the size becomes sufficient for dropping by gravity.

  In the present invention, the metal material may be composed of a simple metal element, an alloy, or a combination of different metal elements, or the metal material may be a powder of the same metal material or a different metal element. The powder is mixed at a predetermined composition ratio and stoichiometric ratio, and is formed into a rod shape by pressure compression or sintering in a heated state, or a processed body obtained by cutting the formed rod into a predetermined shape and processing it, Provided is a method for producing metal particles, wherein the metal particles are continuously or intermittently supplied into the sealed container.

  According to the present invention, the metal material is formed in a structure in which wires of different metal elements are wound together, and the metal element wire is made thicker with a low melting point metal element and thin with a high melting point metal element. Thus, a method for producing metal particles characterized in that a difference in molten state due to a difference in melting point is adjusted is provided.

  In the present invention, the diameter of the metal particles produced by controlling the diameter of the metal particles to be melted and dropped into particles by adjusting the light heating by the light superheated melting and dropping means is adjusted. A metal particle manufacturing method is provided.

  The present invention is also characterized in that the metal particles are manufactured by any one of the above metal particle manufacturing methods.

  As described above, the present invention concentrates on a metal material to form a light heating portion, melts the metal material by light heating, rotates and holds the molten metal at an adjacent molten metal holding portion, and The heating temperature is made uniform, and the holding is continued until it reaches the size of dropping as metal particles by gravity without contact, so there is no contamination of the molten metal and thermal shock for light intensive heating Therefore, it is possible to maintain and maintain a melting temperature and a melting time sufficient to obtain a uniform structure, for example, an intermetallic compound or alloy having a uniform structure.

  In addition, since it is possible to ensure the holding of the melting temperature and the melting time as described above, it is only necessary to supply a wire or an elongated rod as the starting metal material, and it is easy to adjust the starting material and is suitable for mass production. A manufacturing apparatus or a metal particle manufacturing method can be provided.

  Hereinafter, an embodiment of the present invention will be described with reference to the drawings.

  FIG. 1 shows the configuration of a metal particle manufacturing apparatus according to an embodiment of the present invention. In FIG. 1, a metal particle manufacturing apparatus 100 is a glass tube 2 that can be connected to another sealed container as a sealed container, a lamp 3 that is disposed in close proximity to the glass tube 2, and a collection formed around the lamp 3. It is composed of an optical mirror 4. A through hole 29 is formed at the upper end of the glass tube 2, and the metal material 1 is supplied from the through hole 29 to the inside of the glass tube 2. The metal material 1 is slowly rotated by a metal material supply device (not shown) that slowly rotates the metal material. And the metal raw material 1 is supplied continuously or intermittently by the said supply apparatus. Here, the slow rotation of the metal material effectively acts on the homogenization of the structure of the metal particles described later.

  The condensing mirror 4 is configured so that the tilt can be adjusted by a tilting device (not shown). The light emitted from the lamp 3 is condensed by the condensing mirror 4 to become the heating light 5 and irradiated to a predetermined portion. A heating range is set at this irradiation point. The metal material 1 supplied from above is light-heated by the light that reaches the heating range and is concentrated. In this way, the lamp condensing heating means 10 is formed.

  The inside of the glass tube 2 is in a vacuum state or an inert gas atmosphere. When an inert gas is used, the inert gas may flow slowly. Slowly means that it does not affect the dropping of metal particles described later.

In the example shown in FIG. 1, the lamp 3 and the condensing mirror 4 are provided outside the glass tube 2. However, a part of the glass tube 2 may be enlarged and provided inside. In this example, the transparent glass tube 2 is opened so that the melted state can be visually confirmed. However, the melted state can be confirmed by other means so that other members, however, materials that do not elute are produced. You may make it comprise.
The metal material 1 is melted by light heating with concentrated light and becomes non-contact metal particles that grow to a size sufficient to be dropped as metal particles by gravity without using a propellant gas. The metal particles grown to a size sufficient to be dropped as metal particles are dropped by gravity, that is, dropped without borrowing the power of the injection gas.

  In this way, the light heating and melting dripping means 11 is formed using the lamp condensing heating means 10 so as to perform the condensing heating adjustment.

FIG. 2 shows the function and action of the light heating melt dripping means 11.
In FIG. 2, the metal material 1 is formed with a light heating portion 12 and a molten metal holding portion 13 formed of molten metal adjacent to the light heating portion 12 at the light end. The light heating portion 12 is a portion where the light end portion of the metal material 1 is melted by light concentrated heating with light. The metal melted by the light intensive heating is non-contacted and held without dropping by an adjacent molten metal holding part in a non-contact and molten state without borrowing the power of other means. By this holding, the heating temperature, that is, the melting temperature is sufficiently uniformed. This holding is not in contact with any other means, and is large enough (weight) to be dropped as metal particles by gravity. Continue until In this dripping, it is desirable that other means, for example, assistance by injection with an injection gas is not required and is not provided. The holding time and the size of the metal particles depending on the holding time are set by adjusting the temperature by light intensive heating. In any case, it is important to hold the molten metal for a predetermined time by the holding force of the adjacent molten portion, and by maintaining the molten state, the metal is homogenized in the rotating state. For example, uniformized intermetallic compounds and alloys are produced.

  In this way, the light source disposed inside or outside the sealed container has a light heating portion that concentrates on the metal material 1 supplied with the light from the light source and performs light heating, and the light heating is performed. A metal material is melted, and the molten metal is held by its holding power at an adjacent molten metal holding portion where no concentrated light heating is performed, and metal particles are dropped by gravity without using a spray gas. Since it becomes sufficiently large, the light heating melt dripping means 11 is constructed so as to continue the rotation holding and thereby make the structure uniform.

  Then, by using this light heating melting dripping means 11, the molten metal is held at the light end of the metal material 1 by the above-mentioned holding force by light heating adjustment, and the holding is continued, and the tissue is made uniform. Then, the size of the metal particles to be dropped in a state where the structure is made uniform is adjusted, and the metal particles having a desired size are dropped and solidified to form metal particles having a desired size.

  In the present embodiment, the desired size of the metal particles is about 0.2 to 5 mm, and preferably 0.2 to 0.5 mm or 1 to 3 mm according to the purpose of use.

  In the present embodiment, since it is not intended to form a powder or fine particles, the generated molten metal is not separated from the metal material immediately after the generation by a propellant gas or by other means.

  FIG. 3 shows another example. This is basically the same as the example shown in FIGS. 1 and 2, and the same numerals are assigned to the same components. The difference from the previous example is that a laser heating means 10 ′ is used instead of the lamp condensing heating means 10. The laser heating means 10 ′ includes a laser light source 3 </ b> A, and the heating light 5 is generated.

  Also in this example, a light source arranged inside or outside the sealed container has a light heating portion that performs light heating by concentrating on the metal material with light from the light source, and the metal material is formed by light heating. Molten and hold the molten metal in the adjacent molten metal holding part, uniformize the heating temperature of the molten metal part, and keep holding until it reaches the size of dropping as metal particles by gravity without contact The light heating melt dropping means 11 for forming a molten particulate body with the dropped metal particles is constituted.

  In the example shown in FIG. 4, the metal particle collecting part 21 is connected to the lower part of the glass tube 2 as another sealed container using the examples shown in FIGS. 1 and 2. The metal particle collecting unit 21 includes a metal particle cooling unit 22 and a metal particle collecting unit 23. The metal particle cooling part 22 is connected to the lower part of the glass tube 2, bent in one direction (left direction in the figure), and inclined to cool the dropped metal particles 6. And the fall part of the metal particle 6 inclines and is comprised so that an impact may be reduced. The metal particles 6 that have collided with the falling portion and have fallen in speed are collected as metal particles 24 as a product by the metal particle accumulation unit 23.

  As described above, the optically heated floating zone melting apparatus and method according to this embodiment are configured. As the metal material 1 to be supplied, a wire or an elongated rod can be used, and mass productivity can be improved. The homogenization of the metal particle structure and particle size control are performed according to the optical heating conditions depending on the heating temperature corresponding to the metal material supply rate and the shape of the metal material, but the metal material shape and supply rate are constant. In some cases, the temperature is controlled depending on the heating temperature.

  And the holding | maintenance continuation time as the light heating part 12 is determined corresponding to this heating temperature. As the supplied wire or elongated rod-shaped metal material 1, a metal element alone, an alloy, or a material processed by combining different metal elements so as to have a desired metal particle composition ratio can be used.

  FIG. 5 shows the metal material used. Fig.5 (a) shows the metal raw material 31 comprised only with the metal element.

  FIG. 5B shows an example in which metal materials 32 and 33 having the same diameter made of two kinds of metal elements are combined into one metal material 34. FIG. 5C shows a metal material 37 in which metal materials 36 having different diameters composed of two kinds of metal elements are combined and a metal material 36 is arranged at the center. FIG. 5D shows a metal material 38 formed by molding metal element particles.

  In the present embodiment, these metal materials can be used, but are not limited to these metal materials.

  The metal material has a structure in which wires of different metal elements are combined so that a desired metal particle composition ratio is obtained, and the metal element wire has a relatively low melting point metal element and a high melting point metal element thin. By doing so, you may enable it to adjust the difference in a molten state by the difference in melting | fusing point.

  Alternatively, the metal material may be processed into a wire or rod shape by combining metal element particles alone, alloy particles, or different metal element particles so as to have a desired metal particle composition ratio.

  In other words, the metal material is a simple combination of metal elements, an alloy or a combination of different metal elements, or the metal material is a powder of the same metal material or a powder of a different metal element in a desired composition / ratio Mixing so that the desired composition ratio / stoichiometric ratio is achieved in the stoichiometric ratio, pressing and compressing or sintering in a heated state to form a rod, or cutting the molded rod into a predetermined shape It can consist of a body.

  In the above-mentioned example, the production means and method of AlTi metal particles have been shown. According to this example, Al-based intermetallic compounds (aluminides) include Si-based intermetallics such as AlFe, A13Nb, A13Ni2, AlNi, and AlZr3. As the compound (silicide), SI2Cr, Si2Mo, Si2Nb, Si2Ta, Si2Ti, and the like can be applied to NiTi, NiSn, and Ni7Zr2.

  Further, in the Be-based intermetallic compound (berylide), Be12Ti, Be17Ti2, Be3Ti, Be2Ti, Be12V, Be2V, Be12Cr, Be2Cr, Be12Mn, Be13Ba, Be12Fe, Be11Fe, Be7Fe, Be22Ni4, Be21Ni5, BeZr3, BeZr, Be27r, Be12Nb, Be17Nb2, Be3Nb, Be2Nb, Be2Nb3, Be12Ta, Be17Ta2, Be3Ta, Be2Ta, Be2Ta3, BeTa2, Be22Mo, Be12Mo, Bw2Mo, BeMo3, Be22W, Be12

  Further, by using this method, it is possible to synthesize alloys of ternary system or higher including binary systems.

  φ2mm AlTi (Al / Ti = 35 / 65wt%) alloy wire is used as the metal material, and the metal material is heated at an Ar gas flow rate of 20sccm with a rod rotation speed of 20rpm. Heat up to 1600 ° C at 100 ° C / min, melt and drop, and continuously supply the metal material to the heated part at a rate of 10 mm / min while adjusting the lamp output to keep the temperature 1600 ° C constant. The molten metal was kept rotating for a predetermined time, melted and dropped by its own gravity without using a propellant gas in a non-contact manner, and metal particles having an average particle diameter of 3 mm were produced. FIG. 6 is a metal material, and FIG. 7 is a result of 2θ / θ scan X-ray diffraction (XRD) of the produced metal particle, which shows that the AlTi metal material has the same structure and is a metal particle. FIG. 8 shows a photograph of the produced pebble.

  A metal material (Al / Ti == 99.9% purity) and Ti wire (purity 99.9% or more) with a diameter of 0.5 mm, each wire being twisted by 8 wires. 37.5 / 62.5 wt%), using Ar gas flow rate 20 sccm, rod rotation speed 20 rpm, halogen lamp to heat the metal material to 1200 ° C. at a heating rate of 100 ° C./min. To prevent melting and dropping of only the melting point element Al, hold the temperature for 5 minutes, then heat to 1800 ° C. to melt and drop the metal material, and then adjust the lamp output to keep the temperature constant at 1800 ° C. 1 mm The metal material is continuously supplied to the heated part at a speed of / min, and the molten metal is kept rotating at this temperature for a predetermined time, and melted and dropped by its own gravity without using a propellant gas. To obtain metal particles similar average particle diameter 3mm and FIG. FIG. 9 is an X-ray diffraction result of the produced pebble, which is the same as FIG. 7 in the case of using an AlTi alloy wire, and shows that the same metal particles as in Example 1 are formed. A scanning electron microscope (SEM) photograph obtained when the metal particle cross section is enlarged 3000 times and a surface analysis result (element distribution of Al and Ti) by energy dispersive X-ray analysis (EDX) are shown in FIG. a) is an SEM photograph, FIG. 10 (b) is an EDX-Al element distribution, FIG. 10 (c) is an EDX-Ti element distribution), and the peak profile of the element identified by EDX plane analysis and the result. The obtained abundance ratio of Al and Ti is shown in FIG. From these results, segregation or the like was not observed in the element distribution of Al and Ti, and it was shown that particles of the compound dissolved uniformly were formed.

  Using φ2mm Ti wire (purity 99.9% or more) as a metal material, heating up to 1800 ° C under the same conditions as in Example 1, melting and dropping, and then lamp output to keep the temperature constant at 1800 ° C The metal material is continuously supplied to the heated portion at a speed of 10 mm / min while adjusting the temperature, the molten metal is kept rotating at this temperature for a predetermined time, and is shown in FIG. Metal particles having a uniform structure with an average particle diameter of 3 mm as shown in a metal particle photograph were obtained. FIGS. 13 and 14 show the X-ray diffraction results of the Ti wire metal material and the produced pebble, and show that the same peak is formed and the same metal particles as the Ti wire metal material are formed.

FIG. 15 shows the flow of the embodiment of the present invention.
Light heating concentrated on the metal material is performed to form a light heating portion (S1). The metal material is melted by light heating (S2), and the molten metal is held by the adjacent molten metal holding portion (S3). The heating temperature of the molten metal, that is, the melting temperature is made uniform (S4). Next, the metal particles are kept in contact with each other in a non-contact manner without using a propellant gas until the particles are sufficiently dropped by gravity (S5). The generated metal particles are dropped by gravity without using a propellant gas in a non-contact manner (S6), cooled (S7) to form a molten particulate matter (S8), and recovered (S9).

  According to the present embodiment, since a floating zone melting method that does not use a melting container such as a crucible is used, it is possible to prevent impurities from being mixed from the melting container during the production of metal particles, and to control the melting atmosphere. It is possible to produce metal particles having a structure with uniform purity, and it is also possible to observe from the outside during melting, so that the molten state can be easily controlled. Especially when producing heat-resistant particles such as intermetallic particles, not only alloyed metal materials that are difficult to adjust, but also metal that combines wires of metal elements to achieve the required metal particle composition ratio Since it is possible to use a raw material or a metal material formed by molding metal element particles, a manufacturing method with high mass productivity can be provided.

The figure which shows the structure of the Example of this invention. The figure explaining the function of the Example of this invention, an effect | action. The figure which shows the structure of the other Example of this invention. The figure which shows the structure of the other Example of this invention. The figure which shows the example of the metal raw material used by a present Example. The figure which shows an AlTi metal raw material XRD result. The figure which shows the AlTi metal particle XRD result. The figure shown by the AlTi metal particle photograph. The figure which shows the AlTi metal particle XRD result. The figure which shows AlTi metal particle SEM and EDX result. The figure which shows the analysis result by an EDX surface analysis. The figure shown by Ti metal particle photograph. The figure which shows Ti metal raw material XRD result. The figure which shows Ti metal particle XRD result. The flowchart figure of the Example of this invention.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Metal material, 2 ... Glass tube (sealed container), 3 ... Lamp, 3A ... Laser light source, 4 ... Condensing mirror, 5 ... Heating light, 6 ... Dropping metal particle, 10 ... Lamp condensing heating means, 10 ' DESCRIPTION OF SYMBOLS Laser heating means, 11 ... Light heating melt dripping means, 12 ... Light heating part, 13 ... Adjacent molten metal holding part, 21 ... Metal particle collection part, 22 ... Metal particle cooling part, 23 ... Metal particle accumulation part, 24 ... Metal particles as products, 29 ... Through holes, 100 ... Metal particle manufacturing equipment.

Claims (2)

A metal material made of a combination of two types of wires made of metals with different melting points is heated while rotating in an inert gas atmosphere, and at a temperature at which a metal having a lower melting point than the other metal does not melt and drop for a certain period of time A method for producing metal particles, comprising: holding and homogenizing a molten metal, heating to a higher temperature, and melting and dropping the metal material by gravity to produce metal particles. 2. The metal particle manufacturing method according to claim 1, wherein the low melting point metal is Al, the other metal is Ti, and the temperature at which the low melting point metal is not melted and dropped is 1200 ° C. A high temperature is 1800 degreeC, The metal particle manufacturing method characterized by the above-mentioned.

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