JPH0672241B2 - Mechanical alloying device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to a mechanical alloying apparatus for ball-milling a plurality of types of metal powder to alloy them.

(Prior art) Liquid quenching method and sputtering method have been widely used as a method for forming an amorphous alloy, but recently, the formation of an amorphous phase by a mechanical alloying method utilizing solid phase diffusion has attracted attention. ing. This mechanical alloying method is a method in which mechanical energy is added to metal powder by a method such as a ball mill for alloying. Conventionally, a normal ball mill device has been used as a device for this purpose, and no special ball mill device has been developed in consideration of various conditions for mechanical alloying. Therefore, the metal powder to be alloyed and the hard spheres for ball milling are evacuated in a separate glove box or filled with an inert gas, and then vibrated for machining. In addition, no consideration was given to the cooling of heat generated during processing.
After performing ball milling for a certain period of time, the machining was stopped for a certain period of time. Therefore, there is a problem that the working time is long and the sample may be oxidized. Further, since the vacuum pump for evacuating the inside of the container is separate from the ball mill device, there is a drawback that the device occupies a large area and is difficult to move.

(Problems to be Solved by the Invention) As described above, the conventional mechanical alloying device is merely a diversion of a ball mill device, and has not been considered as a dedicated device. Therefore, there are problems that the sample is oxidized, the working time is long, and the apparatus is large.

The present invention has been made in view of the above circumstances, and provides a mechanical alloying device having a compact structure with good operability, which is capable of forming an amorphous alloy in a short time while preventing oxidation and temperature rise of a sample. The purpose is to do.

[Structure of the Invention] (Means for Solving the Problems) In order to achieve the above object, the present invention stores a plurality of types of metal powder and a plurality of hard balls in a closed container, and vibrates the container. In a mechanical alloying device that forms an amorphous alloy, a mounting base supported by an elastic member in a housing, a motor fixed to the mounting base, and a rotation supported by the mounting base and rotated by the motor. A tilted shaft that is driven and has its tip tilted at a predetermined angle, a vibration plate that is swingably supported by a tip of this tilted shaft via a bearing and has the container attached thereto, and a flexible member provided in the housing. The container is provided with a supply of various gases and a vacuum pump through a tube and a valve.

Further, this container is composed of an outer container, an inner container, and a housing, the outer container is fixed to a diaphragm, and the inner container is detachably attached to the outer container. Further, cooling means or heating means is provided between the inner container and the outer container.

Further, one end of the flexible tube may be connected to the inner container, and the other end may be connected to a vacuum pump and a supply source of active gas or inert gas.

(Operation) According to the above configuration, the ball milling can be performed while vacuuming the metal powder contained in the container, or in various gas atmospheres or in a flow state. Further, by cooling or heating the container, the sample can be maintained at an appropriate temperature and a good amorphous alloy can be continuously formed in a short time. Furthermore, by configuring the container with an outer container and an inner container, it is possible to transport and store the inner container containing the metal powder while maintaining a vacuum or gas atmosphere, and prevent oxidation of the metal powder or alloy. it can.
Moreover, since the vacuum pump is provided in the housing, the apparatus has a compact structure and is easy to carry.

Embodiment An embodiment of the mechanical alloying device according to the present invention will be described below with reference to the drawings.

1 to 4 show an embodiment of the present invention. In FIGS. 1 and 2, legs 2 are provided at four corners of the lower surface of the housing 1, and a pair of ribs 3 are integrally formed in parallel on opposite surfaces inside the upper part. Four corners of a mounting base 5 are mounted on the ribs 3 via vibration-proof rubbers 4 so as to be vertically movable. A bearing 6 is provided at the center of the mount 5, and a tilt shaft 7 is rotatably supported by the bearing 6 in a direction perpendicular to the mount 5. An inclined portion 7a that is inclined at a predetermined angle with respect to the axial direction is provided at the tip protruding upward from the. A bracket 8 is fixed to the lower surface of the mounting base 5 at a right angle to the mounting base 5, and a bearing 9 for rotatably supporting the vicinity of the lower end of the tilt shaft 7 is attached to the lower end of the bracket 8.
Is provided. A pipe 10 is mounted between the outer rings of the bearings 6 and 9 so as to maintain the gap between the bearings 6 and 9. A motor 12 is fixed to the side surface of the bracket 8 via a motor base 11. The drive shaft 13 of the motor 12 and the lower end of the tilt shaft 7 are respectively provided with pulleys.
14, 15 are attached, and a belt 16 is stretched between these pulleys 14, 15 so that the rotation of the drive shaft 13 of the motor 12 is transmitted to the tilt shaft 7.

On the other hand, the center of the diaphragm 18 is rotatably mounted on the inclined portion 7a at the tip of the inclined shaft 7 through a bearing 17 at a right angle to the inclined portion 7a. A spring shaft 19 is provided so as to project from each of the two opposite sides. And, one end of each of two springs 20 is locked to each of the spring shafts 19.
The other ends of the diaphragms are respectively locked near the four corners of the mounting base 5, and elastically position and hold the diaphragm 18 with respect to the mounting base 5. Further, the diaphragm 18 has a collar 21 for the inclined portion 7a.
Also, the nut 22 prevents the container from coming off in the axial direction, and the container 23 is attached on the vibration plate 18 at a position symmetrical with respect to the inclined portion 7a. Further, the top of the housing 1 is covered with a cover 24, and a vacuum pump 25 is provided in the housing 1.

Next, the structure of the container 23 will be described with reference to FIGS. 3 and 4. The container 23 is composed of an outer container 26 and an inner container 27 each formed of stainless steel or the like in a cylindrical shape with a bottom, and a lid body 28 also formed of stainless steel or the like in a disk shape. The outer diameter of the inner container 27 is substantially equal to the inner diameter of the outer container 26, and the inner container 27 is detachably fitted in the outer container 26. Further, on the upper end surface of the inner container 27, the collar portion 27a faces outward.
Are integrally formed, and the collar portion 27a is concentrically provided with four mounting holes 29 and four screw holes 30 alternately at equal pitches. Further, on the upper end surface of the outer container 26, four screw holes 31 are provided at positions aligned with these mounting holes 29. Further, the lid 28 is also provided with eight mounting holes 32 at positions aligned with the mounting holes 29 and the screw holes 30 provided in the flange portion 27a of the inner container 27. Then, the bolts 33 are inserted and screwed into the mounting holes 32 and the screw holes 30 of the inner container 27 to fix the lid body 28 to the inner container 27, and the mounting holes 32 of the lid body 28 and the mounting holes of the inner container 27. By inserting the bolt 34 through 29 and screwing into the screw hole 31 of the outer container 26, the lid 28, the inner container
The outer container 27 and the outer container 26 are integrally fixed.
An O-ring 35 is mounted between the end surface of the outer container 26 and the inner surface of the collar portion 27a of the inner container 27, and an O-ring 36 is mounted between the outer surface of the collar portion 27a and the lid 28. There is. Further, the outer container 26 is attached to the diaphragm 18 by a plurality of bolts 37.

On the other hand, a cooling water passage 38 that communicates in the axial direction and the radial direction is formed between the outer container 26 and the inner container 27, and this cooling water passage 38 is connected to the cooling water passage 39 formed in the vibration plate 18. It is in communication. The cooling water passage 39 is connected to a cooling water supply source (not shown) via a port 40 formed on the outer circumference of the diaphragm 18. A two-way needle valve 41 is attached to the center of the lid 28, and the needle valve 41 communicates with a port 42 provided inside the inner container 27 and on the outer circumference of the lid 28.
The port 42 is connected to a piping manifold 44 provided in the housing 1 via a flexible tube 43, and the piping manifold 44 further includes a flexible tube 45 and opening / closing valves 50, 51.
Is connected to the intake port of the vacuum pump 25 and the gas supply port 52 via.

In FIG. 2, reference numeral 46 is an inverter for controlling the rotation of the motor 12, reference numeral 47 is a hinge serving as a fulcrum for opening and closing the cover 24, reference numeral 48 is a stopper for locking the rotation of the diaphragm 18, and reference numeral is shown.
Reference numeral 49 is a vibration-proof rubber attached to the diaphragm 18 and engaged with the stopper 48.

Next, the operation of this embodiment will be described. A plurality of types of metal powder for forming an amorphous alloy and a large number of steel balls formed of stainless steel having a diameter of 11 mm, for example, are housed in the inner container 27, and a lid 28 is attached and fastened with bolts 33. . Next, the inner container 27 is fitted and mounted in the outer container 26, and is integrally fastened and fixed by the bolts 34. Further, the outer container 26 to which the lid 28 and the inner container 27 are fixed is fastened and fixed to the diaphragm 18 with bolts 37, and the port 42 provided in the lid 28 and the piping manifold 44 are connected by the flexible tube 43. . At this time the piping manifold
44 and the vacuum pump 25 are connected to the flexible tube 45 via the opening / closing valve 50.
Connected by. At the same time, it is connected to various gas supplies via the on-off valve 51. Next, after opening the needle valve 41, the vacuum pump 25 is driven to open the opening / closing valve 50 to bring the inside of the container into a vacuum state. After that, the opening / closing valve 50 is closed and the opening / closing valve 51 is filled with gas to close the needle valve 41. The cover 24 covers the upper part of the housing 1 to drive the motor 12. As a result, the vibration plate 18 is locked against rotation by the stopper 48, and the inclined portion 7a of the inclined shaft 7 is
It swings due to its swinging motion. On the other hand, the cooling water is injected from the port 40 formed in the vibration plate 18, and the cooling water passage 3
Since it flows through 9,38, the container 23 is cooled. Therefore, the temperature rise of the container 23 due to the ball milling can be suppressed, and the sample can be maintained at a predetermined temperature to form a good amorphous alloy.

On the other hand, since the container 23 is rocked in an eccentric state, the vibration energy causes the mounting base 5 to vibrate via the vibration isolating rubber 4, and ball milling can be efficiently performed. In addition, this vibration energy changes the rotation speed of the motor 12 into the inverter.
It can be arbitrarily selected by switching under the control of 46. In addition, the amorphous alloy formed in the inner container 26 can be removed from the outer container 26 while being sealed with the lid 28 while maintaining the gas atmosphere, transported and stored, and oxidation can be prevented for a long time.

According to this embodiment, ball milling can be performed in a gas atmosphere, and the temperature rise of the sample can be prevented by cooling with water. Therefore, oxidation of the sample can be prevented and a good amorphous alloy can be obtained. Moreover, since the sample can be transported and stored while maintaining the gas atmosphere in the inner container 27, the sample can be further prevented from being oxidized for a long period of time. Further, since the vacuum pump 25 is housed in the housing 1, the device becomes compact, and installation and transportation are easy.

In the above embodiment, the case where ball milling is performed with the inner container 27 in a gas atmosphere has been described. However, since the container and the vacuum pump are constantly connected by a flexible tube, ball milling is performed even when the container is constantly evacuated. I can do things. Further, by attaching two needle valves 41 to the lid of the container, gas can be supplied and discharged, and gas can be circulated to perform ball milling in a gas flow. Further, the container 23 can be covered with a heater to be heated, or the container 23 can be cooled by circulating liquid nitrogen.

[Effects of the Invention] As described in detail above, according to the mechanical alloying device of the present invention, metal powder and hard balls are hermetically housed in an inner container, and vacuuming or gas filling is performed while cooling or heating. Since the ball mill processing is performed by using the ball mill, it is possible to prevent oxidation of the sample, form a good amorphous alloy, and improve the operability and downsize the apparatus.

[Brief description of drawings]

1 is a front view showing an embodiment of the present invention, FIG. 2 is a plan view of the same, FIG. 3 is a longitudinal sectional view showing the container of FIG. 1, and FIG.
The figure is also a plan view. 1 ... Case, 4 ... Anti-vibration rubber (elastic member) 5 ... Mounting base, 6 ... Bearing 7 ... Tilt shaft, 12 ... Motor 18 ... Vibration plate, 23 ... Container 25 ... Vacuum Pump, 26 …… Outer container 27 …… Inner container, 28 …… Lid body 38,39 …… Cooling water passage (cooling means) 41 …… Needle valve, 43,45 …… Flexible tube 50,51 …… Open / close valve

Claims (4)

[Claims] 1. A mechanical alloying apparatus for accommodating a plurality of kinds of metal powder and a plurality of hard spheres in a hermetically sealed container and vibrating the container to form an amorphous alloy. Mounted mount, a motor fixed to the mount, a tilt shaft rotatably supported by the mount and driven to rotate by the motor, and a tip inclined at a predetermined angle, and a tip of the tilt shaft. A vibration plate, which is swingably supported via bearings and to which the container is attached, and a vacuum pump, which is provided in the housing and is connected to the container via a flexible tube and a valve, are provided. A characteristic mechanical alloying device. 2. The container is composed of an outer container, an inner container and a casing, the outer container is fixed to a vibrating plate, and the inner container is detachably mounted on the outer container. ) The mechanical alloying device described. 3. The mechanical alloying device according to claim 1, wherein the inner peripheral surface of the outer container is provided with cooling means or heating means. 4. One end of the flexible tube is connected to an inner container, and the other end is connected to a vacuum pump and an active gas or inert gas supply source to allow the gas to flow to enable a ball mill in a gas flow. The mechanical alloying device according to claim 1, characterized in that