JPH02263902A - Mechanical alloying apparatus - Google Patents

Abstract

PURPOSE:To prevent oxidation of metal powder and to form a good amorphous alloy by hermetically containing the metal powder and hard balls in a vessel and executing ball mill working while evacuating. CONSTITUTION:The vessel 23 hermetically containing plural kinds of the metal powder and the hard balls is fixed to an oscillating plate 18 and connected with a vacuum pump 25 through flexible tubes 43, 45, etc., to make the vacuum condition in the vessel. By driving a motor 12, the oscillating plate 18 is shaked with shaking movement of inclining part 8a in an inclining shaft 7 while being prevented to rotate with a stopper (not shown in the figure). On the other hand, as the vessel 23 is oscillated under eccentric condition, a fitting table 5 is oscillated through elastic member 4 with this oscillating energy and the ball mill working can be efficiently executed.

Description

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

(Prior art) Liquid quenching and sputtering methods have traditionally been widely used as means for forming amorphous alloys, but recently the formation of amorphous phases by mechanical alloying methods that utilize solid-phase diffusion has attracted attention. ing. This mechanical alloying method is a method in which mechanical energy is applied to metal powder using a method such as a ball mill to effect alloying. Conventionally, a normal ball mill device has been used as a device for this purpose, and a dedicated ball mill device that takes into account the various conditions for mechanical alloying has not been developed. For this reason, the metal powder to be alloyed and the hard balls for ball milling are placed in a separate glove box, the inside of which is evacuated or filled with inert gas, and then processed by vibration.

Furthermore, no consideration has been given to cooling the heat generated during processing, and in the past, in order to prevent the temperature of the sample from rising, ball milling was performed for a certain period of time and then processing was stopped for a certain period of time. Therefore, there are problems in that the work takes a long time and there is a risk that the sample may be oxidized. Furthermore, since the vacuum pump for evacuating the inside of the container was separate from the ball mill device, there were also disadvantages in that the device occupied a large area and was difficult to move.

(Problems to be Solved by the Invention) As described above, the conventional mechanical alloying device is simply a repurposed ball mill device, and no consideration has been given to making it a dedicated device.

This may result in oxidation of the sample, increased working time, or
There were problems such as the equipment becoming larger.

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 and capable of forming an amorphous alloy in a short time while preventing oxidation of the sample and temperature rise. The purpose is to

[Structure of the Invention] (Means for Solving the Problem) 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. A mechanical alloying device for forming an amorphous alloy includes a mounting base supported through an elastic member within a housing, a motor not fixed to the mounting base, and a UgJ
A tilted shaft with a rolling drive and whose tip is tilted at a predetermined angle,
A diaphragm is rotatably supported at the tip of the tilted shaft via a bearing, and the container is attached to the diaphragm, and various gases are supplied to the container through flexible tubes and valves provided inside the housing, and vacuum is supplied to the container. It is equipped with a pump.

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, a cooling means or a heating means is provided between the inner container and the outer container.

Alternatively, 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 source of active gas or inert gas.

(Function) According to the above configuration, ball milling can be performed while the metal powder stored in the container is being evacuated, or in various gas atmospheres or in a flow state. Furthermore, 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 constructing the container with an outer container and an inner container, the inner container containing the metal powder can be transported and stored while maintaining a vacuum or gas cloud atmosphere, thereby preventing oxidation of the metal powder or alloy. I can do it.

Furthermore, since the vacuum pump is provided within the housing, the device has a compact structure and is easy to transport.

(Example) Hereinafter, an example of a mechanical alloying device according to the present invention will be described with reference to the drawings.

An embodiment of the present invention is shown in FIGS. 1 to 4.

In FIGS. 1 and 2, legs 2 are provided at each of the four corners of the lower surface of the housing 1, and legs 2 are provided on the opposing surface inside the upper part.
A pair of ribs 3 are integrally formed in parallel. The four corners of a mounting base 5 are vertically movably housed on these ribs 3 via anti-vibration rubber 4, respectively. A bearing 6 is provided at the center of the mounting base 5, and a tilting shaft 7 is rotatably supported by the bearing 6 in a direction perpendicular to the mounting base 5. An inclined portion 7a that is inclined at a predetermined angle with respect to the axial direction is provided at the tip of the tip 5 that projects upwardly. A bracket 8 is fixed to the lower surface of the mount 5 at a right angle to the mount 5, and a bearing 9 is provided at the lower end of the bracket 8 to rotatably support the vicinity of the lower end of the inclined shaft 7. . And these bearings 6,
A pipe 10 is installed between the outer rings of the bearings 6 and 9.
It is designed to maintain an ra7 spacing of 9. Further, a motor 12 is connected to the side surface of the bracket 8 via a motor stand 11.
is fixed, a pulley 4.15 is attached to the lower end of the drive shaft 13 of the motor 12 and the tilting shaft 7, respectively, and a belt 16 is stretched between these pulleys 14.15. The rotation of the drive shaft 13 of the motor 12 is caused by the tilt axis 7.
It is intended to be transmitted to

On the other hand, the center of a diaphragm 18 is rotatably mounted on the inclined portion 7a at the tip of the inclined shaft 7 via a bearing 17 at right angles to the inclined portion 7a. A spring $1119 is provided to protrude from each of the two opposing sides. One end of two springs 20 is fixed to each of the spring shafts 19, and the other ends of these springs 20 are respectively fixed near the four corners of the mounting base 5, and the diaphragm 18 is fixed to the mounting base. 5
It is elastically positioned and held. Also, diaphragm 1
8 is prevented from coming off in the axial direction with respect to the inclined portion 7a by a collar 21 and a nut 22, and a container 23 is mounted on the diaphragm 18 at a position symmetrical to the inclined portion 7a. Furthermore, the upper part of the housing 1 is covered with a cover 24, and a vacuum pump 25 is provided inside the housing 1.

Next, the structure of the container 23 will be explained with reference to FIGS. 3 and 4. The container 23 is composed of an outer container 26 and an inner container 27, each of which is made of stainless steel or the like in a cylindrical shape with a bottom, and a lid 28 which is also made of stainless steel or the like and has a disc shape. The outer diameter of the inner container 27 is approximately equal to the inner diameter of the outer container 26, and the inner container 27 is removably fitted into the outer container 26.

Further, a flange portion 27a is integrally formed on the upper end surface of the inner container 27 toward the outside, and this flange portion 27a has four mounting holes 29 and four screw holes 30 concentrically arranged at equal intervals. They are arranged alternately with pitches. Additionally, four screw holes 3 are provided on the upper end surface of the outer container 26 at positions that align with these mounting holes 29.
1 is provided. Furthermore, eight attachment holes 32 are provided in the lid body 28 at positions that align with the attachment holes 29 and screw holes 30 provided in the flange portion 27a of the inner container 27. The lid 28 is fixed to the inner container 27 by inserting and screwing the bolts 33 into these mounting holes 32 and the screw holes 30 of the inner container 27, and the inner container 27 is attached to the mounting holes 32 of the lid 28 and the inner container 27. Insert the bolt 34 through the hole 29 and remove the outer container 2.
By screwing into the screw holes 31 of No. 6, the lid body 28, the inner container 27, and the outer container 26 are fixed together. In addition, the end face of the outer container 26 and the flange 27a of the inner container 27
An O-ring 35 is attached between the inner surface of the flange 27a and the inner surface of the flange 27a.
An O-ring 36 is installed between the outer surface of the storage body 28 and the storage body 28, respectively. Furthermore, the outer container 26 has a plurality of bolts 37.
is attached to the diaphragm 18 by.

On the other hand, a cooling water passage 83B communicating in the axial and radial directions is formed between the outer container 26 and the inner container 27, and this cooling water passage 38 connects to a cooling water passage 39 formed in the diaphragm 18. It's communicating. This cooling water passage 39 is connected to a cooling water supply source (not shown) via a boat 40 formed on the outer periphery of the diaphragm 18.

Further, a bitter needle valve 41 is attached to the center of the lid body 28, and this needle valve 41 communicates with a boat 42 provided inside the inner container 27 and on the outer periphery of the lid body 28.

The boat 42 is connected to the housing 1 via a flexible tube 43.
It is connected to a piping manifold 44 provided in
Furthermore, the piping manifold 44 is connected to the intake port of the vacuum pump 25 and the gas supply port 52 via a flexible tube 45 and on-off valves 50, 51.

In FIG. 2, reference numeral 46 is an inverter that controls the rotation of the motor 12, reference numeral 47 is a hinge that serves as a fulcrum for opening and closing the cover 24, reference numeral 48 is a stopper that stops the rotation of the diaphragm 18, and reference numeral 49 is a diaphragm. It is a vibration isolating rubber attached to the stopper 18 and engaged with the stopper 48.

Next, the operation of this embodiment will be explained. A plurality of types of metal powder for forming an amorphous alloy and a large number of steel balls made of stainless steel with a diameter of 11 mm, for example, are stored in the inner container 27, and the lid body 28 is installed and fastened with bolts 33. Fix it. Next, this inner container 27 is fitted into the outer container 26 and fastened and fixed together with bolts 34. Furthermore, the lid body 28
The outer container 26 to which the inner container 27 is fixed is fastened and fixed to the diaphragm 18 with bolts 37, and the boat 42 provided on the lid body 28 and the piping manifold 44 are connected with a flexible tube 43. At this time, the piping manifold 44 and the vacuum pump 25 are connected by a flexible tube 45 via an on-off valve 50. At the same time, it is also connected to various gas supplies via an on-off valve 51. Next, after opening the needle valve 41, the vacuum pump 25 is driven, and the on-off valve 50 is opened to bring the inside of the container into a vacuum state. Thereafter, the on-off valve 50 is closed, gas is filled with the on-off valve 51, and the needle valve 41 is closed. The upper part of the housing 1 is covered with a cover 24, and the motor 12 is driven. As a result, the diaphragm 18 is oscillated by the oscillating movement of the inclined portion 7a of the inclined shaft 7, while its rotation is stopped by the stopper 48.

On the other hand, cooling water is injected from the port 40 formed in the diaphragm 18 and flows through the cooling water passages 39 and 38, so the container 2
3 is cooled. Therefore, the container 23 by ball milling
temperature rise can be suppressed, and a good amorphous alloy can be formed by maintaining the sample at a predetermined temperature.

On the other hand, since the container 23 is oscillated in an eccentric state, the mounting base 5 is vibrated by the vibration energy through the vibration isolating rubber 4, and ball milling can be carried out efficiently.

Further, this vibration energy can be arbitrarily selected by changing the rotation speed of the motor 12 under control of the inverter 46. Further, the amorphous alloy formed in the inner container 26 can be removed from the outer container 26 and transported and stored while being sealed with the lid 28 and maintaining the gas atmosphere, and oxidation can be prevented over a long period of time.

According to this example, ball milling can be performed in a gas atmosphere, and the temperature of the sample can be prevented from increasing by water cooling, so 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 inside the inner container 27, oxidation of the sample can be further prevented for a long period of time. Further, since the vacuum pump 25 is housed within the housing 1, the device becomes compact and easy to install and transport.

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

[Effects of the Invention] As explained in detail above, according to the mechanical alloying device according to the present invention, metal powder and hard balls are hermetically stored in the inner container, and vacuuming or gas filling is performed while cooling or heating. Since the ball milling is carried out using the same method, oxidation of the sample can be prevented and a good amorphous alloy can be formed, and the operability can be improved and the apparatus can be made more compact.

[Brief explanation of drawings]

FIG. 1 is a front view showing one embodiment of the present invention, FIG. 2 is a plan view, FIG. 3 is a vertical sectional view showing the container of FIG. 1, and FIG.
The figure is also a plan view 91... Housing 4.
・・Vibration-proof rubber (bullet 1 component) 5・Mounting base 6・
... Bearing 7 ... Inclined shaft 12 ... Motor 18 ... Vibration plate 23 ... Container 25 ... Vacuum pump
26...Outer container 27...Inner container 28...
Lid bodies 38, 39...Cooling water passage (cooling means) 41...
・Needle valve 43.45...Flexible tube 50
, 51... Opening/closing valve agent Patent attorney Book 1) Takashi

Claims (4)

[Claims] (1) In a mechanical alloying device that stores multiple types of metal powder and multiple hard balls in a sealed container and vibrates the container to form an amorphous alloy, the metal powder is supported within the housing via an elastic member. a mounting base, a motor fixed to the mounting base, a tilted shaft that is rotatably supported by the mounting base and rotationally driven by the motor and whose tip is inclined at a predetermined angle, and a bearing at the tip of the tilted shaft. a diaphragm that is swingably supported through the diaphragm and to which the container is attached;
A mechanical alloying device comprising: a vacuum pump provided within the housing and connected to the container via a flexible tube and a valve. (2) The container is composed of an outer container, an inner container, and a casing,
2. The mechanical alloying device according to claim 1, wherein the outer container is fixed to the diaphragm, and the inner container is detachably attached to the outer container. (3) The mechanical alloying device according to claim (1) or (2), wherein a cooling means or a heating means is provided on the inner peripheral surface of the outer container. (4) One end of the flexible tube was connected to the inner container, and the other end was connected to a vacuum pump and an active gas or inert gas supply source to allow gas to flow and enable ball milling in a gas flow. Claim (1) or (2) characterized by
Or the mechanical alloying device described in (3).