JP2001107113A - Manufacure of metal glass ball, metal glass ball manufactured thereby, and manufacturing device thereof - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a metal glass ball, and a method and a device for manufac turing the metal glass ball in which the grain size of individual particles can be extensively and artificially controlled, and the metal glass ball close to the true sphere and controlled in grain size can be stably mass-produced. SOLUTION: In this metal glass ball manufacturing method, a molten metal melted in a container having a heater is ejected toward a recovery part having an inert atmosphere located therebelow as its droplets by a piston connected to a piezoelectric actuator to generate a specified displacement from orifices in an orifice plate having a plurality of the orifices, and cooled at the cooling speed not less than a critical cooling speed in the inert gas atmosphere of the recovery part.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing metallic glass (amorphous alloy) spheres, particularly metallic glass spheres having a uniform particle size, and metallic glass spheres produced by this method. , And an apparatus for manufacturing the same.

[0002]

2. Description of the Related Art Fine particles of uniform size, that is, fine monodisperse particles, are in increasing demand today in various fields of science and technology. For example, latex particles produced by the sol-gel method, which are well known as fine monodisperse particles, have a standard deviation of the particle size (particle size) distribution of about 10% of the average particle size.
And used as standard size particles in electron microscopic observation. In the semiconductor industry, spherical solder powder having a uniform particle size (particle size) of 30 μm to 40 μm is required for miniaturization and bonding of IC chips. Also, the HI of the alloy powder
Also in P molding, it is said that spherical powder having a uniform particle size (particle size) is necessary in order to prevent the formation of non-uniform voids that are fatal defects for the material.

[0003] As a method for producing fine monodispersed particles, the above-mentioned sol-
There is a gel method, while a plasma rotating electrode method (PREP method) is used if particles of 100 μm or more are desired. If a certain degree of particle size (particle size) is allowed,
A method of mechanically classifying general atomized powder with a sieve or the like is also practical.

However, in the conventional method, it is generally difficult to widely control the particle size, that is, to obtain monodisperse particles having a desired particle size. As described above, the sol-gel method is limited to the preparation of fine particles of 0.1 μm to 1.2 μm. In the PREP method, the production limit is about 100 μm due to the rotational stability of the electrode. To expand the field of application of monodisperse particles at present,
There has been a demand for the development of a production process capable of more freely controlling the particle size (particle size).

[0005] For this reason, the present applicant has filed Japanese Patent Application No. 3-31.
No. 7096, "Method and apparatus for producing spherical monodisperse particles"
(See Japanese Patent Application Laid-Open No. 6-184607), the particle size (particle size) of each particle can be artificially controlled in a wider range, and a spherical particle having a uniform particle size (particle size) closer to a true sphere can be obtained. A method and an apparatus for producing spherical monodisperse particles capable of stably producing dispersed particles have been proposed.

According to this technique, a pulse pressure is generated in a piezoelectric actuator, the pulse pressure is transmitted to a diaphragm via a transmission rod, and further transmitted to a molten metal in close contact with the diaphragm. Due to the displacement not less than the critical displacement to the molten metal, the molten metal is ejected from the orifice provided in the container for storing the molten metal into the inert gas flow one by one as monodisperse particles to be spherical, and the molten metal is made spherical in the cooling water. It is intended to provide a method for producing spherical monodisperse particles, wherein spherical monodisperse particles are collected after cooling, and an apparatus for producing spherical monodisperse particles embodying this method.

[0007]

The method for producing spherical monodisperse particles according to the above-mentioned prior application and the apparatus for producing spherical monodisperse particles embodying this method are capable of producing spherical monodisperse particles with high precision. However, since the number of orifices for ejecting spherical monodisperse particles is one, there is room for improvement in terms of suitability for mass production. The present invention further improves the above-described method and apparatus for producing spherical monodisperse particles to form a form suitable for mass production of spherical monodisperse particles, and also enables production of high melting point metallic glass spheres. is there.

[0008] That is, an object of the present invention is to provide a metallic glass which can control the particle size (particle size) of individual particles more broadly and artificially and has a uniform particle size (particle size) and is closer to a true sphere. It is an object of the present invention to provide a method for producing metal glass spheres capable of stably mass-producing spherical monodisperse particles made of the above, a metal glass sphere produced by this method, and an apparatus for producing the same.

[0009]

In order to achieve the above object, a method of manufacturing a metallic glass sphere according to the present invention comprises the steps of: (a) melting a molten metal (molten metal) in a vessel provided with a heating device; A recovery unit having an inert atmosphere for spheroidizing the droplet located below the droplet by a piston connected to a piezoelectric actuator that generates a predetermined displacement from the orifice of the provided orifice plate. And cooling at a cooling rate higher than the critical cooling rate in the inert gas atmosphere of the collecting section to collect.

Further, the metallic glass sphere according to the present invention is a metallic glass sphere produced by the above-mentioned production method, wherein the variation in diameter between the metallic glass spheres is within ± 10% and substantially monodispersed. It is a particle. Still further, the metallic glass sphere according to the present invention is characterized in that the variation of the diameter of each metallic glass sphere is within ± 2%.

Further, the apparatus for manufacturing a metallic glass sphere according to the present invention comprises a molten metal container for storing molten metal, a heating device provided on an outer periphery of the molten metal container, and a bottom formed on the molten metal container. A nozzle having a cavity formed therein (molten metal reservoir), an orifice plate provided in the nozzle and having an orifice for ejecting the molten metal in the cavity as droplets, and a piezoelectric element generating a predetermined displacement. An actuator, a transmission rod for transmitting the displacement of the piezoelectric actuator to the nozzle as a displacement of a piston inserted into the nozzle, and a cooling rod for cooling the droplet positioned below the orifice plate and forming the droplet into a sphere. A recovery unit having an inert gas atmosphere, wherein the displacement of the piezoelectric actuator causes the transmission rod, piston and Characterized by injecting the droplets into an inert gas in the recovery part of the molten metal from the orifice through the cavity of the nozzle portion in the pulse pressure corresponding to the displacement.

Here, the orifice plate preferably has a plurality of orifices. Further, it is preferable that a precision positioning means for the piston is provided. Preferably, the orifice (inner surface) is made of a material having poor wettability with molten metal.
Further, it is preferable that the heating device includes a carbon susceptor and a work coil.

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an apparatus for producing spherical monodisperse particles according to the present invention will be described in detail based on a preferred embodiment shown in the accompanying drawings. Needless to say, the present invention is not limited to the illustrated example.

FIG. 1 is a schematic side view showing the overall configuration of a metal glass ball manufacturing apparatus (hereinafter, also simply referred to as the present apparatus) 10 according to one embodiment of the present invention. In FIG. 1, reference numeral A denotes a lifter for moving a part of a piston position adjusting mechanism B and a part (a part from a piezoelectric actuator to a nozzle part) of a metal glass sphere forming part C to be separated upward by inspection for inspection and the like. , A motor-driven screw jack. B indicates a piston position adjusting mechanism for finely adjusting the initial position of the piston of the metallic glass ball forming unit C described later.

C is a metal glass sphere forming part which is a main part of the apparatus, D is a collecting part of the completed metal glass sphere, and E is this collecting part D and the above-mentioned metal glass sphere forming part. F is a vacuum suction mechanism used when replacing the periphery of C with an inert gas. F is a cooling water circulating device that supplies cooling water to a cooling mechanism for preventing an excessive rise in temperature of the piezoelectric actuator of the metallic glass ball forming unit C. G is a high-frequency induction heating device for supplying power to the high-frequency heating device of the metallic glass sphere forming section C, H is a power supply box of the entire apparatus, and I is an operation panel for operating the entire apparatus. I have.

FIG. 2 shows the piston position adjusting mechanism B described above.
FIGS. 3 and 4 are enlarged cross-sectional views of a heating device and a nozzle portion, which are main parts of the metal glass sphere forming section C. FIG.

First, the piston position adjusting mechanism B is shown in FIG.
As shown in the figure, an adapter 15 for holding parts such as the piezoelectric actuator 12, the holder block 39, the transmission rod 14, and the piston 14a of the metallic glass ball forming part C.
Holding the adapter 15 and the base flange 13
And two guide shafts 13 also fixed to the base flange 13
b.

The elevating base 31 can be moved up and down along a screw shaft 13a and a guide shaft 13b via a worm gear unit 13c by turning a handle 13d disposed at one end thereof. The initial position (standby position) of the piston can be finely adjusted with an accuracy of, for example, about 0.1 mm. Reference numeral 33 denotes a dial gauge for position reading.

Next, the schematic structure of the metallic glass ball forming section C will be described. In FIG. 2, reference numeral 12 denotes a piezoelectric actuator held by the adapter 15 of the piston position adjusting mechanism B, and reference numeral 14 denotes a transmission rod fixed to the piezoelectric actuator 12 by a holder block 39. The tip of the rod 14 forms a piston 14a that is inserted into a nozzle 25 described later. An intermediate portion of the transmission rod 14 (a portion between the connection portion to the piezoelectric actuator 12 and the base flange 13) is covered with a bellows 23 having elasticity in order to prevent intrusion of foreign matters and the like.

On the base flange 13, a raw material supply port 60a through which the raw material supply pipe 60 is inserted, and an insertion port 61 of a thermocouple 62 for temperature measurement are provided. A nozzle holder 46 described below is fixed to the lower side of the base flange 13, and a crucible 26 and a nozzle unit 25 described later are also held by the nozzle holder 46. Nozzle 25 from below base flange 13
The space up to is also a part for sending the raw material supplied from the raw material supply pipe 60 to a heating device 20 described below therebelow.

As shown in FIG. 3 in detail, the heating device 20 includes a quartz crucible 26 for holding the heated and melted raw material together with the nozzle portion 25. A carbon susceptor 20a made of carbon, which is a heating element, and a heat insulating material 20b arranged so as to surround these components. And a protection tube 20c on the outside thereof, and a work coil 20d for high-frequency heating disposed outside the protection tube 20c. Further, a lid 21 for heat insulation is provided at an upper portion of the heating device 20.

The above-described heating device 20 excites the work coil 20d by the excitation current supplied from the high-frequency induction heating device G shown in FIG. 1, and heats the carbon constituting the carbon susceptor 20a by the high frequency generated from the work coil 20d. The heat is used to heat and melt the crucible 26 inside the carbon susceptor 20a and the raw metal charged therein, and has excellent uniform heating characteristics. This has the advantage that it can be easily obtained. The heating device 20 is also effective when using a raw material that does not generate heat even when a high frequency is applied directly.

The nozzle portion 25 is set inside (below) the crucible 26 whose outer periphery is supported by the crucible 26.
On the upper surface, as shown in FIG. 4, an inverted conical recess 25a for bringing a molten raw material (hereinafter, referred to as molten metal) to a central portion of the nozzle portion 25, and for feeding the molten metal to an orifice portion described later. And a plurality of nozzles 25b. The nozzle 25b communicates with a space 25c in the nozzle portion 25 below the piston 14a (this is a substantial melt storage portion, hereinafter referred to as a cavity). It is stored in the cavity 25c via the nozzle 25b.

On the lower surface of the nozzle portion 25, an orifice plate 27 having a number of orifices for spraying metallic glass is provided.
Are attached by a pressing member 27a. As the material constituting the orifice plate 27, an optimum material may be selected according to the type of the target metallic glass. For example, the wettability with the molten metal can be changed by selecting the material. . Also, the diameter of the orifice is not particularly limited, and may be appropriately selected according to the particle diameter of the sphere to be produced. For example, it is preferably about 30 μm to 500 μm, more preferably about 50 μm to 150 μm.

The upper part of the nozzle part 25 continues to the crucible 26 provided with a thermocouple 62 for temperature measurement.
As described later, a raw material supplied is melted, and a raw material melting portion and a molten metal reservoir for storing the molten raw material are formed. Below the raw material melting portion and the molten metal reservoir, a substantial molten metal reservoir (cavity) further below the piston 14a that is kept inserted into the nozzle portion 25 via the nozzle 25b in the nozzle portion 25. 25c is as described above.

Above the crucible 26, a reflector 45 for maintaining the temperature in the crucible 26 and preventing the heat from being released to the outside is disposed over the raw material supply port 60a. The reflector 45 has thin metal plates on the upper and lower sides, and both are connected by a wire-like connecting member. Needless to say, the reflector 45 is provided with a hole for inserting the transmission rod 14 and the piston 14a and a hole for passing the raw material supplied from the raw material supply pipe 60.

The crucible 26, the nozzle portion 25, the reflector 45, and the like are locked by the nozzle holder 46 provided with the above-described material supply port 60a and the thermocouple insertion port 61. Are lifted out of the heating device 20 by the lifter A at the time of inspection or the like.

On the other hand, below the orifice plate 27 of the nozzle section 25, there is provided a collecting section (D in FIG. 1) for catching the injected metallic glass sphere. The recovery section D has a sample tray 40 for capturing an initial injection sample at the uppermost stage, a recovery cylinder 41 to which an inert gas flow is supplied below, a gate valve 42, and a recovery cylinder 41 after being injected. A product (metallic glass ball) collection box 43 and the like cooled inside are connected.

The collecting section composed of these parts includes:
A vacuum suction mechanism E used to replace the surroundings of the collecting section D and the metallic glass sphere forming section C with an inert gas is connected, and the above-described gate valve 42 is turned on in a preparation stage before the apparatus is driven. In the open state, the inside of the collection section D and the periphery of the metal glass sphere forming section C are evacuated by the vacuum suction mechanism section E, and after the evacuation, an inert gas such as helium gas is supplied from a supply source (not shown) at a predetermined pressure. And the entire path of the metallic glass sphere is made to have an inert gas atmosphere.

The sample tray 40 receives the metallic glass spheres which are ejected at the beginning of the operation of the apparatus, and observes the situation by using a metal microscope, for example.
It is for confirmation. In this state, the cooling is not performed sufficiently, so that agglomeration / deformation occurs and a glass bulb having a perfect shape cannot be obtained. However, it is possible to sufficiently confirm the suitability of the manufacturing conditions. The sample tray 40 is configured to retreat from the main passage at the time when the confirmation of the appropriateness of the manufacturing conditions is completed.

In the recovery section D, an inert gas atmosphere is formed by an inert gas to promote the spheroidization of the molten metal (molten metal) sprayed from the orifice in the form of droplets, as will be described later. . That is, here, the inert gas is controlled so as to have an optimum cooling rate for spheroidizing the metallic glass. In the present apparatus, a cooling rate of about 1000 ° C./sec can be realized in a helium gas atmosphere, depending on the particle size. Needless to say, such an inert gas atmosphere also has an effect of preventing oxidation of the metal glass spheres, and brings about an effect on the production of high quality metal glass spheres.

The inert gas atmosphere is not particularly limited as long as the control of the cooling rate of the droplet is optimal for spheroidization, and the type of metal glass, the temperature, the injection speed, and the diameter of the orifice ( That is, the diameter of the metal glass sphere)
What is necessary is just to select suitably according to various parameters. Also,
The length of the collecting portion D, that is, the length of the metallic glass sphere injected from the orifice in the inert gas, is not particularly limited, and is appropriately determined according to the above parameters, the type and the flow rate of the inert gas, and the like. do it.

As the piezoelectric actuator 12 used in the metallic glass ball forming section C, a laminated piezoelectric element (for example,
AE0505D16 manufactured by Tokin Corporation: Maximum displacement 1
4.7 μm, frequency characteristics 1.7 MHz) can be suitably used. The piezoelectric actuator 12 is connected to a function generator that generates a rectangular wave of a predetermined frequency and a power amplifier (both not shown) that amplifies the rectangular wave, and applies a rectangular wave generated and amplified by these. Thus, the displacement of the predetermined frequency is generated.

The above displacement is caused by the piezoelectric actuator 1
2 through a transmission rod 14 fixed to the piston 1
4a. The piston 14a is inserted into the nozzle portion 25, and a cavity 25 in the nozzle portion 25 is provided.
By transmitting the displacement to the molten metal stored in c, the molten metal is ejected from the orifice at a pulse pressure corresponding to the displacement to produce fine metallic glass balls.

The piezoelectric actuator 12 is attached to the holder block 39 by, for example, an actuator retainer fixed by four set screws (not shown) screwed into four screw holes on the side surface thereof. Can be The connection between the piezoelectric actuator 12 and the transmission rod 14 is performed by sandwiching the piezoelectric actuator 12 between the actuator retainer and the transmission rod 14 and fixing the actuator retainer and the transmission rod 14 with bolts and nuts.

As described above, since the piezoelectric actuator 12 and the transmission rod 14 are integrally formed, the movement of the piezoelectric actuator 12 can be accurately transmitted to the piston 14a. Accordingly, it is possible to accurately vibrate. Also,
With such a configuration using the piezoelectric actuator 12, accurate displacement control of the piston 14a, high-speed driving (it can follow high-frequency pulses), and control with an arbitrary waveform are possible.

In general, a piezoelectric element is required to be cooled because its piezoelectric function is impaired at a high temperature. For this reason, also in the device 10 according to the present embodiment, the cooling water circulation device E as shown in FIG. 1 is used, and the water cooling pipe is partially connected to the device main body (the piezoelectric actuator 12 and the holder block 3).
9 and the like, so as to maintain the piezoelectric actuator 12 at a temperature lower than its use limit temperature.

In addition, above the heating device 20, an inert gas introduction pipe 35 connected to a supply source (not shown) is provided.
Is arranged, and the atmosphere in the crucible 26 is adjusted separately from the atmosphere adjustment of the entire metal glass sphere forming section C described later. This is because the balance between the pulse pressure wave applied to the molten metal corresponding to the displacement transmitted to the piston 14a and the stable formation of good glass spheres is maintained. Control the supply, crucible 2
The control of the gas pressure in 6 (and the gas pressure applied to the cavity 25c) is performed.

The raw material that can be produced by the apparatus for producing metallic glass spheres according to the present invention is not particularly limited, and various kinds of materials such as palladium, zirconium, and lanthanum can be produced. Can be used in combination. Therefore, the temperature of the molten metal is not particularly limited as long as it is not lower than the melting point of the raw material metal used and the required fluidity can be obtained.

In the present apparatus 10, the piezoelectric actuator 12 displaces (vibrates) the piston 14a toward the molten metal, so that a plurality (many) of metal glass balls are ejected from the orifice by one displacement (vibration). Thus, a metal glass sphere having a diameter substantially equal to the diameter of the orifice is obtained. Here, the displacement of the piston 14a is
Needless to say, it is necessary to correspond to the total volume according to the diameter and the number of the metallic glass spheres to be injected.

The frequency of the displacement of the piezoelectric actuator 12 is not particularly limited, and may be appropriately selected according to the type of the target metallic glass sphere (material), the required production speed, and the like. As for the above-mentioned target materials, for example, about 10 Hz to 1 KHz can be practically used. It is needless to say that this frequency is preferably as high as possible from the viewpoint of mass productivity of the metallic glass sphere.

Hereinafter, the operation of the apparatus 10 for manufacturing metallic glass spheres according to this embodiment configured as described above will be described with reference to the drawings.

First, the raw material of the metallic glass sphere to be manufactured is charged into the crucible 26 from the raw material supply pipe 60, and the power of the heating device 20 is turned on to melt the charged raw material. The molten raw material (melt) accumulates on the nozzle portion 25 at the bottom of the crucible 26, and partly fills the cavity 25c through the nozzle 25b described above by reciprocating the piston 14a up and down several times. Is done. In addition, after the raw material is melted, the heating device 20 may be kept warm.

On the other hand, the cooling water supplied from the cooling water circulating device E is circulated through the holder block 39 and the like so that the temperature of the piezoelectric actuator 12 does not rise. Further, the air around the metallic glass sphere forming section C and the collecting section D are exhausted using the vacuum suction mechanism section E, and an inert gas is supplied from a supply source (not shown).
An inert gas atmosphere slightly higher than the atmospheric pressure is set.

Next, a rectangular wave of a predetermined frequency is generated by the above-described function generator, amplified by a power amplifier, and applied to the piezoelectric actuator 12 to generate a vibration of a predetermined frequency and a predetermined amplitude. Then, the piston 14a is oscillated with a pulse having the same frequency as above via the transmission rod 14 having an integral structure, and a pulse pressure wave is generated in the molten metal in the cavity 25c in contact with the piston 14a.

Thus, when the piezoelectric actuator 12 is displaced downward by a predetermined displacement amount or more, the piston 14a is displaced via the transmission rod 14, and the molten metal in the cavity 25c is changed from the orifice on the orifice plate 27 into droplets. To inject. This injection is performed once per cycle of the pulse pressure wave. At this time, the molten metal flows in and out of the cavity 25c through the nozzle 25b of the nozzle portion 25 in response to the vibration of the piston 14a, so that the inert gas pressure in the crucible 26 above the nozzle portion 25 is reduced by the vibration of the piston 14a. It is preferable to precisely control the balance in forming the metallic glass sphere.

The cooling rate of the droplets thus jetted is optimally controlled by the inert gas atmosphere in the collecting section D.
While descending in the collecting section D, it is made into a spherical shape almost near a true sphere, and collected as a metallic glass sphere. Thus, it is possible to obtain a metallic glass sphere having a diameter close to the diameter of the substantially orifice and having a spheroidized shape substantially close to a true sphere. The particle size (particle size) distribution of the metallic glass spheres thus obtained has very little variation.

[0048]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The above-mentioned laminated piezoelectric element (AE0505D16 manufactured by Tokin Co., Ltd.) was used as the piezoelectric actuator 12, and a personal computer and a D were used as pulse wave generators.
A board MDA-761AT (manufactured by NF Circuit Design Block Co., Ltd.), NF-4025 (power company) as a power amplifier
NF circuit design block). The maximum displacement of the laminated piezoelectric element used as the piezoelectric actuator 12 is 14.7 μm, and the frequency characteristic is 1.7 MHz.

Here, cooling water was passed through a water cooling pipe to cool the piezoelectric element so as not to reach 40 ° C. or higher. High temperature members (actuator retainer 40, transmission rod 1
4. The nozzle part 25 and the like were made of ceramic. The orifice plate 27 is also made of ceramic, and the piston 1
Sixty orifices were provided within the cross-sectional area of 4a (about 40 mm ² ). The diameter of the orifice was about 400 μm.

As a raw material of the metallic glass sphere, a palladium-based material (Pd-Cu-NI-P: melting temperature of about 900 ° C.)
To 1000 ° C.) and 1000 ° C.
Helium gas was introduced into the collection section D at a pressure of 0.1 atm from an introduction pipe (not shown).
The droplet ejected from the orifice has a diameter of about 50
cm below the product collection box 43 of the collection section D.

The operating frequency of the piezoelectric actuator 12 is set to 1
The apparatus was operated at 00 Hz for 2 minutes to produce metal glass balls. At the initial stage, the droplets ejected from the orifice are set so as to be received by the above-described sample tray 40, and the formation state of the particles is determined by observation with a metallographic microscope, and when it is determined that the droplets are normal, Removed the sample tray 40 and collected the droplets directly below the orifice into the product collection box of the collection section D.

With respect to the metallic glass spheres collected in the product collection box 43, the particle shape was observed with a scanning electron microscope (SEM) and the particle size distribution was measured with an image analyzer. Although not shown, a CCD camera (48 in FIG. 1) is installed in the collection section D to observe the shape of the metallic glass sphere being manufactured in real time.
The production conditions were adjusted based on the observation results.

FIGS. 5A and 5B show SEM photographs of the metallic glass spheres obtained in the above example. FIG. 5 (a)
FIG. 5B shows particles obtained when the injection temperature is 1000 ° C., and FIG. 5B shows particles obtained when the injection temperature is 900 ° C. In the case of the injection temperature of 1000 ° C. shown in FIG. 5A, the particles do not solidify during the fall due to the shortage of the cooling time and are deformed by the impact of the drop, but the injection shown in FIG. Temperature 900
In the case of ° C, particles close to a true sphere were obtained.

FIG. 6 shows the injection temperature 90 shown in FIG.
The particle size distribution of the particles obtained at 0 ° C. is shown. The monodisperse particles obtained in the above example have an average particle diameter of 383.9 μm substantially equal to the orifice diameter (standard deviation 4.1).
7) was spherical particles. The sphericity (variation in the diameter of each metallic glass sphere) was ±, as a result of measurement based on the SEM photograph of the metallic glass sphere shown in FIG.
It was confirmed that it was within 2%.

The variation in size (diameter) between a large number of manufactured metallic glass spheres is at most 10%, preferably at most 5%, more preferably at most 2%. Monodisperse particles can be obtained. Further, the metallic glass sphere manufactured by the present apparatus has a feature that its surface cleanliness is good (that is, the thickness of the oxide film layer is extremely thin).

From these results, the metallic glass spheres obtained by the apparatus for producing metallic glass spheres according to the present embodiment are not only what can be called monodisperse particles, but also have excellent sphericity. It can be said that it has a wide application range. FIG. 7 shows the injection temperature 90 shown in FIG.
The XRD analysis result of the particles obtained at 0 ° C is shown. In FIG. 7, no remarkable peak is observed, and it can be seen that amorphousization has progressed and vitrification has occurred.

Even when the same metallic glass spheres were produced using different raw materials, spherical particles having an average particle diameter substantially equal to the orifice diameter were obtained. The raw material used here was a zirconium-based Zr-Al-Cu-NI (melting temperature of about 950 ° C to 1 ° C).
100 ° C.) and lanthanum-based La-Al-NI-Cu-Co (melting temperature about 400 ° C. to 600 ° C.). The properties of the obtained particles, such as the shape, particle size (particle size) distribution, and vitrification ratio, were the same as those in the previous examples.

According to each of the above-described embodiments, an effect was obtained in which metal glass spheres having an arbitrary particle diameter can be produced at a desired speed from a molten metal glass having a high melting temperature. Note that the above embodiment is an example of the present invention, and it is needless to say that the present invention is not limited to this.

For example, the diameter of the orifice provided on the orifice plate 27 and the number thereof are determined by the diameter of the piston 14a,
It can be selected in a wide range according to the diameter of the metallic glass sphere to be produced and the desired production speed. Also,
The operating frequency of the piezoelectric actuator 12 can be easily set to about 10 Hz to 70 KHz, and the production speed can be controlled also by this.

[0060]

As described in detail above, according to the present invention, the particle size (particle size) of each particle can be controlled more widely and artificially, and the particle size (particle size) is uniform. Thus, there is an effect that a method and an apparatus for manufacturing a metal glass ball capable of stably mass-producing a metal glass ball closer to a true sphere can be realized. Further, according to the above manufacturing method, it is possible to obtain metal glass spheres having high uniform characteristics by using a metal glass having a high melting point as a raw material.

[Brief description of the drawings]

FIG. 1 is a schematic side view showing an overall configuration of a metal glass ball manufacturing apparatus according to one embodiment of the present invention.

FIG. 2 is a schematic sectional view showing a detailed configuration of a piston position adjusting mechanism B and a metal glass sphere forming unit C in FIG.

FIG. 3 is an enlarged cross-sectional view of a heating device, which is a main part of the metallic glass ball forming section C in FIG.

FIG. 4 is an enlarged sectional view of a nozzle portion, which is a main part of the metallic glass ball forming section C in FIG.

FIGS. 5 (a) and 5 (b) are SEM photographs instead of drawings showing the particle structure of the monodisperse particles obtained in one example.

FIG. 6 is a graph showing the particle size distribution of the monodisperse particles shown in FIG. 5 (b).

FIG. 7 is a graph showing an XRD analysis result of the monodisperse particles shown in FIG. 5 (b).

[Explanation of symbols]

 Reference Signs List A Lifter B Piston position adjusting mechanism C Metal glass ball forming unit D Recovery unit E Vacuum suction mechanism F Cooling water circulation device G High frequency induction heating device H Power supply box I Operation panel 10 Metal glass ball manufacturing device 12 Piezoelectric actuator 13 Base flange 14 Transmission rod 14a Piston 20 Heating device 20a Carbon susceptor 20b Heat insulating material 20d Work coil 25 Nozzle part 25b Nozzle 25c Cavity 26 Crucible 27 Orifice plate 27a Pressing member 33 Dial gauge 39 Holder block 40 Sample tray 41 Collection cylinder 42 Gate valve 43 Collection box 45 Reflector 46 Nozzle holder 48 CCD camera 60a Raw material supply port 61 Thermocouple insertion port

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[Procedure amendment]

[Submission date] October 13, 1999 (1999.10.
13)

[Procedure amendment 1]

[Document name to be amended] Drawing

[Correction target item name] Fig. 5

[Correction method] Change

[Correction contents]

FIG. 5

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Ryo Kawasaki, Inventor 5-51-701, Showa-cho, Aoba-ku, Sendai, Miyagi Prefecture (72) Eiichi Makabe 3-1-25 Kutake, Miyagino-ku, Sendai, Miyagi Co., Ltd. Makabe Giken (72) Inventor Shoji Omura 3-1-25-1 Kutake, Miyagino-ku, Sendai-shi, Miyagi F-term (reference) 4K017 AA04 BA02 BA08 BA10 BB01 BB05 BB06 CA01 DA05 EC04 EK02

Claims (7)

[Claims] 1. A piston connected to a piezoelectric actuator for generating a predetermined displacement of molten metal (molten metal) melted in a vessel provided with a heating device from the orifice of an orifice plate having a plurality of orifices. By
As a droplet, the droplet positioned below is sprayed toward a recovery unit having an inert atmosphere for spheroidizing the droplet, and cooled at a cooling rate higher than the critical cooling rate in the inert gas atmosphere of the recovery unit. And producing the metallic glass spheres. 2. A metal glass sphere manufactured by the manufacturing method according to claim 1, wherein a variation in diameter between the metal glass spheres is within ± 10%. 3. The metallic glass sphere according to claim 2, wherein the variation in the diameter of each metallic glass sphere is within ± 2%. 4. A molten metal container for storing molten metal, a heating device provided on an outer periphery of the molten metal container,
A nozzle portion having a cavity (molten metal storage portion) formed at the bottom of the molten metal container, and an orifice plate provided in the nozzle portion and having an orifice for ejecting the molten metal in the cavity as droplets; A piezoelectric actuator that generates a predetermined displacement, and a transmission rod that transmits the displacement of the piezoelectric actuator to the nozzle as a displacement of a piston inserted into the nozzle,
A recovery unit located below the orifice plate and having an inert gas atmosphere for cooling and spheroidizing the liquid droplets, wherein the displacement of the piezoelectric actuator causes the cavities of the transmission rod, the piston, and the nozzle unit Wherein the molten metal is ejected from the orifice through the orifice as droplets into the inert gas of the recovery unit. 5. The apparatus according to claim 4, wherein the orifice plate has a plurality of orifices. 6. The apparatus for manufacturing a metallic glass sphere according to claim 4, further comprising means for precisely positioning the piston. 7. The apparatus according to claim 4, wherein the heating device comprises a carbon susceptor and a work coil.