JP2012160545A - Method for manufacturing hydrogen pulverized powder of raw material alloy for rare-earth magnet, and manufacturing apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for manufacturing a hydrogen pulverized powder of a raw material alloy for a rare-earth magnet, which can adjust oxygen content of the hydrogen pulverized powder, and also can recover the hydrogen pulverized powder after the low oxygen powder to be hydrogen pulverized of which the oxygen content has been adjusted and a normal oxygen powder to be hydrogen pulverized have been subjected to hydrogen pulverization, can add a lubricant to the hydrogen pulverized powder and can mix the hydrogen pulverized powder and the lubricant, in a common container; and to provide a manufacturing apparatus therefor.SOLUTION: The manufacturing method includes the steps of: reducing a pressure in a recovery chamber; subsequently discharging the hydrogen pulverized powder in a treatment container into the recovery chamber; after discharging the hydrogen pulverized powder into the recovery chamber, introducing an inert gas and/or an oxygen-containing gas into the recovery chamber, and setting the inside of the recovery chamber to a predetermined pressure and a predetermined oxygen concentration; subsequently recovering the hydrogen pulverized powder in the recovery container; adding the lubricant to the hydrogen pulverized powder in the recovery container; and then mixing the hydrogen pulverized powder and the lubricant while cooling the recovery container.

Description

  The present invention relates to a method and apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy.

Two types of high-performance rare earth magnets are widely used: samarium / cobalt magnets and neodymium / iron / boron magnets.
In particular, neodymium / iron / boron magnets (hereinafter referred to as “R-T-B magnets”) exhibit the highest magnetic energy product among various magnets and are relatively inexpensive. Has been adopted.
The R-T-B magnet is composed of a main phase mainly composed of a tetragonal compound of R ₂ T ₁₄ B, an R-rich phase, and a B-rich phase. In an R-T-B magnet, the magnetic properties are basically improved by increasing the abundance ratio of the main phase R ₂ T ₁₄ B tetragonal compound. However, R easily reacts with oxygen in the atmosphere, and forms an oxide such as R ₂ O ₃ . Therefore, when the R-T-B magnet raw material alloy and its powder are oxidized during the manufacturing process, the abundance ratio of R ₂ T ₁₄ B is reduced, the R-rich phase is reduced, and the magnetic properties are rapidly reduced. . That is, magnetic properties are improved by preventing oxidation during the manufacturing process and reducing the oxygen content of the raw alloy for the RTB-based magnet and its powder.
The rare earth magnets such as the above-described R-T-B magnets are manufactured through a sintering process and a heat treatment process after press forming an alloy powder formed by roughly pulverizing and finely pulverizing a raw material alloy. In the production of rare earth magnets, hydrogen pulverization is frequently used in the process of coarsely pulverizing a raw material alloy because of high pulverization efficiency.
The hydrogen pulverization is a method of pulverizing the raw material alloy by causing the raw material alloy to absorb hydrogen and embrittle it, and is performed by the following steps.
First, an alloy as a raw material is inserted into a hydrogen furnace, and then the inside of the hydrogen furnace is depressurized by evacuation. Thereafter, hydrogen gas is supplied into the hydrogen furnace, and hydrogen is stored in the raw material alloy (hydrogen storage step). After the elapse of a predetermined time, the raw material alloy is heated while evacuating the hydrogen furnace (heating step), hydrogen is released from the raw material alloy, and then cooled (cooling step) to complete the hydrogen pulverization. As a result, the raw material alloy becomes brittle and becomes coarsely pulverized powder.
The coarsely pulverized powder after hydrogen pulverization (hereinafter referred to as “hydrogen pulverized powder”) is pulverized into a finely pulverized powder of several μm in the subsequent fine pulverization step.
Since rare earth elements themselves are active and oxidize when exposed to the atmosphere, it is effective to improve the magnetic properties of magnets using rare earth elements in order to improve their magnetic properties. ing.

For example, a technology (Patent Document 1) for reducing the oxygen content of a sintered body by directly injecting finely pulverized powder into mineral oil or the like and then molding it. There is a technique (Patent Document 2) in which an agent is added and the surface of particles is coated to prevent oxidation of finely pulverized powder.
In the process of manufacturing rare earth magnets, even in the coarsely pulverized powder of rare earth magnet raw material alloy having relatively large grains, if it is brought into contact with the air in the middle of the process, the oxidation proceeds rapidly and the oxygen content increases. It is known that the magnetic properties of the finally obtained sintered magnet deteriorate.
As a method for obtaining a raw material alloy before rough pulverization of a rare earth magnet, a strip casting method, which is a kind of quenching method, is finally widely used because a sintered magnet having high magnetic properties can be finally obtained. . As another quenching method, a centrifugal casting method has been proposed.

The thickness of the rare earth magnet raw material alloy produced by the rapid cooling method is generally in the range of 0.03 mm to 10 mm. Particularly, in the strip cast method, it is 1 mm or less.
Since the raw material alloy produced by the rapid cooling method is cooled in a relatively short time compared to the raw material alloy produced by the conventional ingot casting method (die casting method), the structure is refined, Small crystal grain size. Further, the total area of the grain boundaries is large, and the dispersibility of the R-rich phase is also excellent.
Moreover, since the raw material alloy by the rapid cooling method is easily broken at the grain boundary by the hydrogen pulverization method, an R-rich phase is likely to appear on the particle surface of the obtained alloy powder. Since R in the R-rich phase easily reacts with oxygen, the raw material alloy powder by the rapid cooling method is very easily oxidized, and the magnetic characteristics are greatly deteriorated.
In order to prevent oxidation of the hydrogen pulverized powder, a technique (Patent Document 3) has been proposed in which a process in a recovery chamber for discharging the hydrogen pulverized powder from the hydrogen pulverizer is performed in an inert gas.

  As proposed in Patent Document 3, the hydrogen pulverized powder can be prevented from being oxidized by being managed in an inert gas. In Patent Document 3, in the recovery chamber for discharging the hydrogen pulverized powder from the hydrogen pulverizer, the recovery process is performed for each transport container storing the hydrogen pulverized powder. That is, the process of dropping the hydrogen pulverized powder in the transport container to the bottom of the collection chamber and discharging the hydrogen pulverized powder from the bottom of the recovery chamber to the collection container is repeated for each transport container. In addition, the transport container from which the hydrogen pulverized powder has been discharged is carried out of the collection chamber. When the transport container is unloaded, the collection chamber is opened to the outside air. The recovery chamber communicated with the outside air is evacuated and inert gas is introduced before a new transfer container is carried in, so oxygen does not exist. Therefore, the hydrogen pulverized powder in the newly carried transport container is not oxidized.

However, if hydrogen pulverized powder remains in the recovery chamber, the remaining hydrogen pulverized powder is oxidized in communication with outside air, and the oxidized hydrogen pulverized powder is mixed into the hydrogen pulverized powder in the new transfer container. Will be. Therefore, in the method disclosed in Patent Document 3, since the hydrogen pulverized powder is discharged from the transport container in an inert gas, the dropped hydrogen pulverized powder may rise and accumulate in the collection chamber and remain. There is.
Although not described in Patent Document 3, in order to collect the accumulated hydrogen pulverized powder without leaving it, it is also possible to drop it with, for example, an air hammer placed on the funnel-shaped part at the bottom of the box-shaped cylindrical container. However, a large-scale device is required, and with only an air hammer, all the hydrogen pulverized powder remaining in places other than the funnel-shaped part, such as the inlet / outlet where the transfer container enters and exits, the transfer device, the upper part of the recovery chamber, etc. is discharged. It is difficult to do.
In this way, the hydrogen pulverized powder remaining in the recovery chamber is gradually oxidized and mixed into the hydrogen pulverized powder to be processed next time. As a result, the oxygen content of the obtained sintered magnet is increased and the magnetic properties are lowered. Invite. For this reason, it is necessary to prevent the mixed hydrogen pulverized powder from being mixed, particularly by eliminating the residual hydrogen pulverized powder in the recovery chamber.

As described above, in the R-T-B magnet, the magnetic properties are improved by reducing the oxygen content of the raw material alloy and powder. Therefore, if the hydrogen pulverized powder is used to prevent oxidation of the finely pulverized powder by the method described in Patent Documents 1 and 2 by using the hydrogen pulverized powder that eliminates residual hydrogen pulverized powder and prevents the mixing of oxidized hydrogen pulverized powder. An RTB-based magnet having excellent magnetic properties with a reduced content can be obtained.
However, in order to prevent oxidation of finely pulverized powder having a small particle size and being easily oxidized, especially after the hydrogen pulverization, a new apparatus or process must be employed as described in Patent Documents 1 and 2. However, there is a problem that the manufacturing cost increases. Further, since the finely pulverized powder is extremely active, there is a possibility that the finely pulverized powder may ignite due to rapid oxidation, and there is a problem that handling is dangerous.
Therefore, in order to improve the safety of handling finely pulverized powder, jet mill pulverization is performed in an inert gas containing a specific amount of oxygen, and an oxide film is formed on the surface of the finely pulverized powder to stabilize the finely pulverized powder. A technique (Patent Document 4) has been proposed. According to this technology, ignition of finely pulverized powder can be prevented, press molding in the air can be performed, the efficiency of press molding can be improved, and an R-T-B magnet can be provided at a low cost. can do.
As described above, in a rare earth magnet, particularly an R-T-B magnet, a magnet with reduced oxygen content and improved magnetic properties (hereinafter referred to as “low oxygen magnet”), and an oxygen content higher than that of the magnet. However, a relatively inexpensive magnet (hereinafter referred to as “ordinary oxygen magnet”) is provided on the market although it has many magnetic properties and is inferior.

  In addition, when producing either the low oxygen magnet or the normal oxygen magnet, fine pulverization is generally performed by jet mill pulverization as in Patent Document 4. In order to prevent adhesion (burn-in) of finely pulverized powder to the interior wall of the jet mill during jet mill pulverization and to improve pulverizability, or between finely pulverized powders or between finely pulverized powder and gold during molding (particularly during dry molding) Molding aids and lubricants (hereinafter collectively referred to as hydrogen pulverized powder) are used to prevent the degree of orientation from decreasing due to friction with the mold wall surface, and to prevent scratches, peeling, and cracks on the mold surface and molded product surface. Techniques for adding and mixing (referred to as “lubricants”) (Patent Documents 5 and 6) are known, and are indispensable steps in recent methods for producing RTB-based magnets.

Japanese Patent No. 2731337 Japanese Patent No. 3418605 JP 2005-118625 A Japanese Patent Publication No. 6-6728 JP-A-5-94922 JP-A-4-191302

In order to manufacture the low oxygen magnet, it is necessary to prepare hydrogen pulverized powder (hereinafter referred to as “low oxygen hydrogen pulverized powder”) having an oxygen content reduced as much as possible. On the other hand, when low oxygen hydrogen pulverized powder is used in manufacturing the normal oxygen magnet, jet mill pulverization is performed in an inert gas containing a specific amount of oxygen as described above, and an oxide film is formed on the finely pulverized powder surface. It is necessary to stabilize the finely pulverized powder, but even if the hydrogen pulverized powder originally having a low oxygen content is jet milled in an inert gas containing a specific amount of oxygen, There is a problem that the formation is not sufficient and cannot be completely stabilized. Therefore, it is necessary to prepare hydrogen pulverized powder for normal oxygen magnets (hereinafter referred to as “normal oxygen hydrogen pulverized powder”) containing a specific amount of oxygen in advance separately from the hydrogen pulverized powder for low oxygen magnets.
Usually, to prepare oxygen hydrogen pulverized powder, it is possible to oxidize low oxygen hydrogen pulverized powder exposed to the atmosphere, but the oxygen content of the obtained hydrogen pulverized powder depends on the state of the exposed atmosphere (seasonal It is not stable because it is affected by changes in room temperature, humidity, or other external environment, and it is difficult to control and stabilize the oxygen content of finely pulverized powder using such hydrogen pulverized powder. .
Therefore, conventionally, these low oxygen hydrogen pulverized powder and normal oxygen hydrogen pulverized powder have been produced by different hydrogen pulverizers.
However, operating a plurality of hydrogen pulverizers causes problems that the manufacturing cost increases and the manufacturing line becomes complicated. In general, in a mass production scale manufacturing process, it is desirable to unify the specifications of equipment used in the process, reduce the cost required for equipment maintenance, and reduce the cost of products.
Thus, it is desirable that the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder are produced using a common hydrogen pulverizer, and this includes a hydrogen pulverizer capable of adjusting the oxygen content of the hydrogen pulverized powder. However, conventionally, such a hydrogen pulverizing apparatus has not been proposed.

  On the other hand, as described above, addition and mixing of the lubricant to the hydrogen pulverized powder is indispensable, and it is necessary to add and mix the lubricant to the low oxygen hydrogen pulverized powder or the normal oxygen hydrogen pulverized powder. In general, the addition and mixing of a lubricant are performed by inserting hydrogen pulverized powder and a lubricant into a closed container such as a V-type mixer and rotating the container for a required time. However, if oxygen is contained in the atmosphere in the container, the hydrogen pulverized powder is gradually oxidized during mixing, and the temperature in the container rises due to the reaction heat. At this time, if a solid (powder) lubricant having a relatively low melting point is used, the lubricant will stick to the inner wall of the container, and the effect of adding the lubricant in the pulverization process or molding process cannot be obtained. is there. Further, there is a problem that the lubricant stuck to the inner wall of the container is peeled off at the time of the next mixing, and remains as a lump and remains as a foreign substance, or is mixed as it is and becomes an added amount more than necessary. In addition, regardless of the presence or absence of oxygen in the container, the temperature in the container also rises due to friction between the hydrogen pulverized powders, resulting in the same problem as described above.

  Therefore, when adding the lubricant to the hydrogen pulverized powder, it is necessary to use a means such as in a container in an atmosphere in which oxygen is removed as much as possible, or to cool the container itself. However, when adding a lubricant to the hydrogen pulverized powder or when transferring the hydrogen pulverized powder to a mixing container, the container must be released, and oxygen cannot be avoided. . In other words, technologies that can collect hydrogen pulverized powder after hydrogen pulverization, add a lubricant to the hydrogen pulverized powder, and mix hydrogen pulverized powder and a lubricant while maintaining an oxygen-free state have been proposed. Not. For this reason, it is desirable to cool the container itself in order to prevent temperature rise in the container, assuming that oxygen is mixed in the container, but a technique of mixing hydrogen pulverized powder and lubricant while cooling the container. Has not been proposed so far.

It is an object of the present invention to reduce the residual hydrogen pulverized powder after hydrogen pulverization in the recovery chamber, and to reduce the oxygen content of the obtained rare earth magnet, thereby improving the magnetic properties. An object of the present invention is to provide a method and apparatus for producing hydrogen pulverized powder of a raw material alloy for a system magnet.
Another object of the present invention is to produce a low-oxygen hydrogen pulverized powder and a normal oxygen-hydrogen pulverized powder using a common hydrogen pulverizing apparatus by adjusting the oxygen content of the hydrogen pulverized powder in the above-described manufacturing method and manufacturing apparatus. Another object of the present invention is to provide a method and apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy.
Another object of the present invention is to recover the hydrogen pulverized powder after hydrogen pulverization of the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder, add a lubricant to the hydrogen crushed powder, hydrogen An object of the present invention is to provide a method and an apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet that can mix pulverized powder and a lubricant in a common container.

  The method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the first aspect of the present invention includes a hydrogen occlusion step of occluding hydrogen in a rare earth magnet raw material alloy accommodated in a processing vessel, and pulverization by hydrogen occlusion. A heating step of heating and dehydrogenating the rare earth magnet raw material alloy, a cooling step of cooling the heated rare earth magnet raw alloy, and hydrogen pulverization of the cooled rare earth magnet raw alloy A recovery step of recovering the powder in a recovery container; a lubricant addition step of adding a lubricant to the hydrogen pulverized powder in the recovery container containing the recovered hydrogen pulverized powder; and the lubricant added A mixing step of mixing the hydrogen pulverized powder and the lubricant while cooling the recovery container containing the hydrogen pulverized powder, and a method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy, wherein the recovery step But before Performed in a recovery chamber connected to one or a plurality of processing chambers for performing a hydrogen storage step, the heating step, and the cooling step, and a first gas introduction means for introducing an inert gas into the recovery chamber; A second gas introduction means for introducing an oxygen-containing gas; a vacuum exhaust means for discharging the gas in the recovery chamber; a carry-in port for carrying the processing container from the processing chamber into the recovery chamber; and the recovery chamber And a recovery container connected to the discharge port, and after introducing an inert gas into the recovery chamber by the first gas introduction means, the processing container is After carrying in from the processing chamber into the recovery chamber through the carry-in port and depressurizing the recovery chamber by the vacuum exhaust means, the hydrogen pulverized powder in the processing container is discharged into the recovery chamber, and the hydrogen crushed powder is In the collection room Then, an inert gas and / or an oxygen-containing gas is introduced into the recovery chamber by the first gas introduction means and / or the second gas introduction means, and the recovery chamber has a predetermined pressure and a predetermined oxygen concentration. Then, the hydrogen pulverized powder is collected in the collection container.

The present invention described in claim 2 is the method for producing hydrogen pulverized powder of the rare earth magnet raw material alloy according to claim 1, wherein the recovery chamber has an inverting means for inverting the processing vessel up and down. The processing container has an opening on an upper surface thereof, and the rare earth magnet raw material alloy in the processing container is discharged by upside down by the inversion means.
According to a third aspect of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the second aspect, the opening is directed downward after performing upside down by the inversion means. In the state, the swinging operation is performed by the reversing means.
According to a fourth aspect of the present invention, in the method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to the second or third aspect, the processing container covers the opening of the processing container. The cover is covered with the lid during decompression by the vacuum evacuation means, and after the decompression means decompresses the collection chamber, the lid is It removes from the said opening part, It is characterized by the above-mentioned.
According to a fifth aspect of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the fourth aspect, the hydrogen is obtained in a state where the opening of the processing vessel is covered with the lid. The occlusion process, the heating process, and the cooling process are performed.
According to a sixth aspect of the present invention, in the method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the first to fifth aspects, the discharge of the hydrogen pulverized powder from the processing vessel is performed. The collection chamber is performed under a reduced pressure of 1000 Pa to 1 Pa.
According to a seventh aspect of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth based magnet raw material alloy according to any one of the first to sixth aspects, the predetermined pressure in the recovery chamber is previously inactivated. The pressure is the same as the pressure in the recovery container in which the oxygen concentration is 20 ppm or less by introducing gas.
The present invention according to claim 8 is the method for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to any one of claims 1 to 6, wherein the predetermined pressure in the recovery chamber is previously inactivated. The pressure is the same as the pressure in the recovery container in which the oxygen concentration exceeds 20 ppm by introducing the gas and / or the oxygen-containing gas.
According to a ninth aspect of the present invention, in the method for producing a hydrogen pulverized powder of the rare earth magnet raw material alloy according to the first aspect, the lubricant has a melting point of 100 ° C. or lower.
According to a tenth aspect of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the first or ninth aspect of the present invention, the addition of the lubricant is disposed in the recovery container. It is characterized by being performed by a bucket.
The present invention according to claim 11 is the method for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of claims 1, 9 and 10, wherein the cooling of the recovery container is recovered. It is characterized by being performed by a water cooling jacket disposed on the outer surface of the container.
A twelfth aspect of the present invention is the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the eleventh aspect of the present invention, characterized in that a coolant of 20 ° C to 30 ° C is supplied to the water cooling jacket. .
A thirteenth aspect of the present invention is the method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the first and ninth to twelfth aspects, wherein the hydrogen pulverized powder and the lubricant Is performed by rotating the collection container itself.

  The apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy of the present invention according to claim 14 comprises subjecting the rare earth magnet raw alloy contained in a processing vessel having an opening on the upper surface to hydrogen storage treatment and heat treatment. One or a plurality of processing chambers for cooling treatment, and a recovery chamber connected to the processing chamber, wherein the recovery chamber includes a first gas introduction means for introducing an inert gas, and an oxygen-containing gas. Second gas introduction means to be introduced, vacuum evacuation means for discharging the gas in the recovery chamber, a carry-in port for carrying the processing container from the processing chamber into the recovery chamber, and a lower portion of the recovery chamber And discharging the hydrogen pulverized powder of the rare earth-based magnet raw material alloy in the processing container carried into the recovery chamber from the processing chamber into the recovery chamber, and from the discharge port to the recovery container Rare earth magnet raw material alloy recovered An apparatus for producing hydrogen pulverized powder, wherein the recovery container is provided with a bucket for storing a lubricant in the recovery container and a water cooling jacket for cooling the recovery container on an outer surface of the recovery container. The recovery chamber includes a reversing means for inverting the processing container upside down, and a pressure measuring means for measuring the pressure in the recovery chamber, and the pressure measured by the pressure measuring means after operating the evacuation means. The reversing means is operated based on the above information, the processing vessel is turned upside down, and the hydrogen pulverized powder of the rare earth magnet raw material alloy in the processing vessel is discharged into the recovery chamber.

The present invention according to claim 15 is the apparatus for producing hydrogen pulverized powder of the rare earth magnet raw material alloy according to claim 14, further comprising oxygen concentration measuring means for measuring the oxygen concentration in the recovery chamber. Features.
According to a sixteenth aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of the rare earth magnet raw material alloy according to the fourteenth or fifteenth aspect, the pressure measured by the pressure measuring means is 1000 Pa or less. It is characterized by.
According to a seventeenth aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to any one of the fourteenth to sixteenth aspects of the present invention, the inversion means inverts the processing vessel upside down. The processing container is further swung with the opening of the processing container facing downward.
The present invention according to claim 18 is the apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of claims 14 to 17, wherein the processing container includes the opening of the processing container. A lid opening / closing means for removing the lid and the lid opening / closing means, and the lid opening / closing means engages the engagement piece provided in the lid and the engagement piece provided in the collection chamber; The lid is removed by upward movement of an engagement piece provided in the collection chamber.
The present invention according to claim 19 is the apparatus for producing hydrogen pulverized powder of the rare earth magnet raw material alloy according to claim 18, wherein the engagement piece provided on the lid is on the upper part of the lid. The engagement pieces provided in the collection chamber are respectively arranged in the upper part of the collection chamber, one of the engagement pieces has a T-shaped cross-sectional shape, and the other engagement piece is substantially C-shaped. It is characterized by having a cross-sectional shape.
The present invention according to claim 20 is the apparatus for producing a hydrogen pulverized powder of a raw material alloy for rare earth magnet according to any one of claims 14 to 19, wherein the recovery chamber is configured to place the processing container in the processing chamber. The reversing means reverses the processing container together with the conveyor means.
According to a twenty-first aspect of the present invention, there is provided the apparatus for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the twentieth aspect of the present invention, on both sides of the conveyer means in the processing container transport direction. Each provided with movement preventing means for preventing movement, and provided on both sides of the conveyor means in a direction perpendicular to the processing container carry-in direction, respectively, with detachment preventing means for preventing separation of the processing container from the conveyor means at the time of reversal, At the time of reversing by the reversing means, the processing container is held at a predetermined position with respect to the conveyor means by the pair of movement preventing means and the pair of separation preventing means.
According to a twenty-second aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the twenty-first aspect, the conveyor means includes a plurality of rollers, and the movement preventing means includes the It is provided so as to be able to appear and retract on the processing container side from between the rollers.
According to a twenty-third aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the twenty-first or twenty-second aspect, the separation preventing means has an L-shaped cross-sectional shape, It arrange | positions so that it may be located in the upper part of the collar part provided in the outer periphery of the said opening part vicinity of a container, It is characterized by the above-mentioned.
According to a twenty-fourth aspect of the present invention, in the apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the fourteenth to twenty-third aspects, the outlet has a valve, and the valve Is composed of an annular expansion member disposed on the inner peripheral surface of the cylindrical member, and a disk member having the radial direction of the cylindrical member as a rotation axis.
According to a twenty-fifth aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the fourteenth aspect, the lubrication is provided in the recovery container by inverting the bucket in the recovery container. It is characterized by discharging the agent.
According to a twenty-sixth aspect of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the fourteenth aspect, a coolant of 20 ° C. to 30 ° C. is supplied to the water cooling jacket on the outer surface of the recovery container. It is characterized by that.

According to the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy of the present invention, when the hydrogen pulverized powder of the rare earth magnet raw material alloy in the processing vessel is discharged into the recovery chamber, the pressure in the recovery chamber is reduced. Therefore, the hydrogen pulverized powder falls without fluttering in the collection chamber, and therefore does not adhere to the wall surface of the collection chamber. Therefore, the hydrogen pulverized powder adhering to the wall surface of the recovery chamber is oxidized when the recovery chamber is opened to the outside air by, for example, carrying out the processing container, and is less likely to be mixed into the hydrogen pulverized powder in the next hydrogen pulverization. Can stably mass-produce low-oxygen hydrogen pulverized powder and improve the magnetic properties of the rare earth magnet.
In addition, when discharging from the discharge port to the recovery container, an inert gas and / or oxygen-containing gas is introduced to bring the recovery chamber to a predetermined pressure, so that smooth discharge can be performed. Therefore, a large-scale device is not required. Moreover, according to the manufacturing method of this invention, the yield of hydrogen pulverized powder can be improved significantly.
In addition, before the hydrogen pulverized powder is collected in the collection container, an inert gas and / or an oxygen-containing gas is introduced into the collection chamber so as to have a predetermined oxygen concentration. The low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder can be produced by using a common hydrogen pulverizing apparatus. Therefore, the manufacturing cost can be reduced, the manufacturing line can be simplified, and the cost required for equipment maintenance can be reduced.
Further, when the lubricant is added to the hydrogen pulverized powder in the collection container, it is not necessary to release the collection container, and oxygen can be prevented from being mixed into the collection container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
In addition, in order to mix hydrogen pulverized powder and lubricant while cooling the recovery container, usually in the atmosphere in the recovery container such as when adding a solid or powdery lubricant with a relatively low melting point to oxygen hydrogen pulverized powder Even if oxygen is contained in the mixture and the hydrogen pulverized powder is gradually oxidized during mixing, the temperature rise in the recovery container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
In this way, the lubricant is added to the hydrogen pulverized powder in the recovery container, and the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. In this case, the hydrogen pulverized powder recovered after hydrogen pulverization, the addition of a lubricant to the hydrogen pulverized powder, and the mixing of the hydrogen pulverized powder and the lubricant can be performed in a common container.

According to the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy of the present invention, the hydrogen pulverized powder of the rare earth magnet raw material alloy contained in a processing vessel having an opening on the upper surface is operated after the vacuum exhaust means is operated. The reversing means is operated based on the pressure information measured by the pressure measuring means, and the processing container is turned upside down and discharged into the collection chamber, so that the hydrogen pulverized powder falls without fluttering in the collection chamber. It does not adhere to the wall surface. Therefore, the hydrogen pulverized powder adhering to the wall surface of the recovery chamber is oxidized when the recovery chamber is opened to the outside air by unloading the processing container, etc. In operation, the low oxygen hydrogen pulverized powder can be mass-produced stably, and the magnetic properties of the rare earth magnet can be improved.
Further, since the processing container is turned upside down by the reversing means, a large amount of hydrogen pulverized powder can be discharged into the collection chamber at a time, so that the time required for collecting the hydrogen pulverized powder can be greatly shortened. Furthermore, since a relatively simple operation of upside down is employed, a large-scale device is not necessary, and the entire collection device can be reduced in size. Moreover, according to the manufacturing apparatus of this invention, the yield of hydrogen pulverized powder can be improved significantly.
Further, after discharging the hydrogen pulverized powder of the rare earth magnet raw material alloy into the recovery chamber and before recovering it in the recovery container, it is inactivated by the first gas introduction means and / or the second gas introduction means in the recovery chamber. By introducing the gas and / or oxygen-containing gas to have a predetermined oxygen concentration, the oxygen content of the hydrogen pulverized powder can be controlled within a desired range. It can be manufactured using a common hydrogen pulverizer. Therefore, the manufacturing cost can be reduced, the manufacturing line can be simplified, and the cost required for equipment maintenance can be reduced.
Moreover, since the bucket for accommodating a lubricant in the collection container is disposed, the lubricant can be added to the hydrogen crushed powder in the collection container. Therefore, it is not necessary to release the collection container, and oxygen can be prevented from being mixed into the collection container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
Further, since the water cooling jacket for cooling the recovery container is provided on the outer surface of the recovery container, the hydrogen pulverized powder and the lubricant can be mixed while cooling the recovery container. Therefore, a small amount of oxygen is contained in the atmosphere in the recovery container, such as when adding a powdery lubricant having a relatively low melting point to oxygen hydrogen pulverized powder. Even if it oxidizes, the temperature rise in the collection container due to the heat of reaction can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
Thus, the recovery container is provided with a bucket for storing the lubricant in the recovery container and a water cooling jacket for cooling the recovery container on the outer surface of the recovery container. In any case of oxygen hydrogen pulverized powder, recovery of hydrogen pulverized powder after hydrogen pulverization, addition of lubricant to hydrogen crushed powder, and mixing of hydrogen pulverized powder and lubricant can be performed in a common container.

1 is a block diagram showing a method for producing a rare earth magnet according to Example 1 of the present invention. Schematic diagram of a rare earth magnet manufacturing apparatus according to Example 1 of the present invention. The front view which shows the outline of the container blender of FIG. FIG. 3 is a partially broken cross-sectional view illustrating the configuration inside the collection container of FIG. The block diagram which shows the collection | recovery process of hydrogen ground powder, the mixing process of hydrogen ground powder, and a wax in the manufacturing method of the rare earth magnet by Example 2 of this invention, and a subsequent process. Schematic configuration diagram of a hydrogen pulverization apparatus for a rare earth magnet raw material alloy according to Example 2 of the present invention Front view of essential parts of recovery chamber (recovery device for hydrogen pulverized powder of rare earth magnet raw material alloy) in the hydrogen pulverizer Side view of the main part of the collection room Fig. 8 is an enlarged view of the main part. Top view of the main part of the collection chamber Configuration diagram showing the operation of the valve provided at the outlet of the recovery chamber

A method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the first embodiment of the present invention includes a hydrogen occlusion step of storing hydrogen in a rare earth magnet raw material alloy accommodated in a processing vessel, and hydrogen occlusion. A heating step of heating and dehydrogenating the pulverized rare earth magnet material alloy, a cooling step of cooling the heated rare earth magnet material alloy, and a hydrogen of the cooled rare earth magnet material alloy A recovery step of recovering the pulverized powder in a recovery container, a lubricant addition step of adding a lubricant to the hydrogen pulverized powder in the recovery container containing the recovered hydrogen pulverized powder, and the lubricant added A method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy comprising a mixing step of mixing the hydrogen pulverized powder and the lubricant while cooling the recovery container containing the hydrogen pulverized powder. Process A first gas introduction means for introducing an inert gas into the recovery chamber, which is performed in a recovery chamber connected to one or a plurality of processing chambers for performing the hydrogen storage step, the heating step, and the cooling step. A second gas introducing means for introducing an oxygen-containing gas, a vacuum exhaust means for discharging the gas in the recovery chamber, a carry-in port for carrying the processing container from the processing chamber into the recovery chamber, A discharge port disposed at a lower portion of the recovery chamber; and the recovery container connected to the discharge port, and after introducing the inert gas into the recovery chamber by the first gas introduction unit, the processing container From the processing chamber into the recovery chamber through the carry-in entrance, and after the pressure in the recovery chamber is reduced by the vacuum exhaust means, the hydrogen pulverized powder in the processing container is discharged into the recovery chamber, and the hydrogen crushed powder The recovery After discharging into the recovery chamber, an inert gas and / or an oxygen-containing gas is introduced into the recovery chamber by the first gas introduction means and / or the second gas introduction means, and the recovery chamber is filled with a predetermined pressure and a predetermined oxygen. After the concentration, the hydrogen pulverized powder is recovered in the recovery container.
Here, the “oxygen-containing gas” refers to, for example, air or a mixed gas of air and an inert gas, or oxygen (100% oxygen) or a mixed gas of oxygen and an inert gas. The “inert gas” refers to a gas having low reactivity such as argon gas, nitrogen gas, helium gas, and the like.

According to the present embodiment, when the hydrogen pulverized powder in the processing container is discharged into the collection chamber, the pressure in the collection chamber is reduced, so that the hydrogen crushed powder falls without flying in the collection chamber. It does not adhere to the wall surface. Therefore, the hydrogen pulverized powder adhering to the wall surface of the recovery chamber is oxidized when the recovery chamber is opened to the outside air by unloading the processing container, etc. In operation, the low oxygen hydrogen pulverized powder can be mass-produced stably, and the magnetic properties of the rare earth magnet can be improved. In addition, when discharging from the discharge port to the recovery container, an inert gas and / or oxygen-containing gas is introduced to bring the recovery chamber to a predetermined pressure, so that smooth discharge can be performed. Therefore, a large-scale device is not required. Moreover, according to this Embodiment, the yield of hydrogen pulverized powder can be improved significantly.
In addition, before collecting the hydrogen pulverized powder into the collection container, an inert gas and / or oxygen-containing gas is introduced into the collection chamber to obtain a predetermined oxygen concentration in the collection chamber, whereby the oxygen content of the hydrogen crushed powder is predetermined. Can be adjusted. For example, if an inert gas is introduced into the recovery chamber, low oxygen hydrogen pulverized powder having a very low oxygen content and suitable for a low oxygen magnet can be obtained. Moreover, if oxygen-containing gas or oxygen-containing gas and inert gas are introduced into the recovery chamber, normal oxygen-hydrogen pulverized powder having an oxygen content suitable for a normal oxygen magnet can be obtained.
Thus, according to the present embodiment, the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder can be produced using a common hydrogen pulverizing apparatus. Therefore, the manufacturing cost can be reduced, the manufacturing line can be simplified, and the cost required for equipment maintenance can be reduced.
In the case where the oxygen content of the hydrogen pulverized powder is adjusted by bringing oxygen into contact with the hydrogen pulverized powder as described above, it is preferable that the hydrogen pulverized powder is sufficiently cooled before the contact with oxygen. By sufficiently cooling the hydrogen pulverized powder, the reaction between the hydrogen pulverized powder and oxygen in the atmosphere can be strictly controlled, and the oxygen content of the hydrogen pulverized powder can be accurately adjusted according to a predetermined value. It becomes.
As the oxygen-containing gas, for example, by using a dry oxygen-containing gas having an atmospheric pressure dew point of −10 ° C. or lower, it is possible to suppress the influence of the moisture contained in the gas on the oxidation of the hydrogen pulverized powder. It is possible to accurately adjust the oxygen content of the hydrogen pulverized powder by a predetermined value.
Further, according to the present embodiment, since the lubricant is added to the hydrogen pulverized powder in the recovery container, it is not necessary to release the recovery container, and oxygen can be prevented from being mixed into the recovery container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
In addition, according to the present embodiment, the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. Therefore, the solid or powdered lubricant having a relatively low melting point such as paraffin wax is usually added to the oxygen hydrogen pulverized powder. Even when an agent is added, even if oxygen is contained in the atmosphere in the recovery container and the hydrogen pulverized powder is gradually oxidized during mixing, the temperature rise in the recovery container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
In this way, the lubricant is added to the hydrogen pulverized powder in the recovery container, and the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. In this case, the hydrogen pulverized powder recovered after hydrogen pulverization, the addition of a lubricant to the hydrogen pulverized powder, and the mixing of the hydrogen pulverized powder and the lubricant can be performed in a common container.
In the present embodiment, the lubricant includes at least one of a hydrocarbon-based lubricant, a fatty acid, or a fatty acid derivative, and a solid, granular, or powdered one can be used. For example, paraffin wax is used as the hydrocarbon-based lubricant, and zinc stearate is used as the fatty acid and / or fatty acid derivative. In particular, according to this embodiment, since the temperature rise in the collection container can be prevented, there is an advantage that paraffin wax or the like having a relatively low melting point can be uniformly mixed with the hydrogen pulverized powder.

The second embodiment of the present invention is a method for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the first embodiment, and the recovery chamber has a reversing means for turning the processing vessel upside down. The processing vessel has an opening on the upper surface, and discharges the rare earth-based magnet raw material alloy in the processing vessel by upside down by an inverting means.
According to the present embodiment, compared with the case where the lower part of the processing container is opened and the hydrogen pulverized powder is dropped, the hydrogen pulverized powder is less likely to remain around the opening and the periphery of the lid, and the pressure is further reduced. Therefore, there is no influence of the rising of the hydrogen pulverized powder due to the generation of the air flow by the reversing operation.

According to the third embodiment of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the second embodiment, the opening portion is turned downward after performing upside down by the inversion means. The swinging operation is performed by the reversing means in the state.
According to the present embodiment, a small amount of hydrogen pulverized powder remaining in the processing container can be completely dropped.

According to a fourth embodiment of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the second or third embodiment, the processing container has a lid that covers the opening of the processing container. When the pressure is reduced by the vacuum evacuation means, the opening is covered with the lid, and after the collection chamber is depressurized by the vacuum evacuation means, the lid is removed from the opening before being turned upside down by the reversing means.
According to the present embodiment, it is possible to prevent the hydrogen pulverized powder from being discharged together with the gas during the decompression operation, and the hydrogen pulverized powder does not rise due to the generation of an air flow when the lid is opened.

According to a fifth embodiment of the present invention, in the method for producing hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to the fourth embodiment, the hydrogen occlusion step is performed with the opening of the processing vessel covered with a lid. A heating process and a cooling process are performed.
According to the present embodiment, the hydrogen storage step, the heating step, and the cooling step can be performed in the state covered with the lid, and the hydrogen pulverized powder is discharged together with the gas at the time of decompression in the recovery chamber. There is no end.

The sixth embodiment of the present invention is a method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to any one of the first to fifth embodiments, wherein the discharge of the hydrogen pulverized powder from the processing vessel is performed, The inside of the recovery chamber is performed under a reduced pressure of 1000 Pa to 1 Pa.
According to the present embodiment, it is possible to eliminate the generation of airflow in the recovery chamber, and it is possible to prevent the hydrogen pulverized powder from adhering to the recovery chamber wall surface and the like.

According to a seventh embodiment of the present invention, in the method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the first to sixth embodiments, the pressure in the recovery chamber is previously set to the inert gas. The oxygen pressure is reduced to 20 ppm or less by introducing the same pressure as the pressure in the recovery container.
According to this embodiment, oxidation in the recovery container can be suppressed, and the hydrogen pulverized powder can be easily discharged from the recovery chamber to the recovery container.

In an eighth embodiment of the present invention, in the method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the first to sixth embodiments, the pressure in the recovery chamber is previously set to an inert gas and / Or the same pressure as the pressure in the recovery container in which the oxygen concentration exceeds 20 ppm by the introduction of the oxygen-containing gas.
According to this embodiment, the oxidation in the recovery container can be controlled, and the hydrogen pulverized powder can be easily discharged from the recovery chamber to the recovery container.

According to a ninth embodiment of the present invention, in the method for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to the first embodiment, the lubricant has a melting point of 100 ° C. or lower.
According to the present embodiment, the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. Therefore, even when a lubricant having a relatively low melting point of 100 ° C. or lower is added to the oxygen hydrogen pulverized powder, Even if oxygen is contained in the atmosphere in the container and the hydrogen pulverized powder is gradually oxidized during mixing, the temperature rise in the collection container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.

According to a tenth embodiment of the present invention, in the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the first or ninth embodiment, the addition of a lubricant is provided in a recovery container. It is done by.
According to the present embodiment, it is not necessary to release the collection container, and oxygen can be prevented from being mixed into the collection container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.

According to an eleventh embodiment of the present invention, in the method for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to any one of the first, ninth and tenth embodiments, the recovery container is cooled. This is performed by a water cooling jacket disposed on the outer surface.
According to the present embodiment, the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container by the water cooling jacket. Even if oxygen is contained in the atmosphere in the recovery container and the hydrogen pulverized powder is gradually oxidized during mixing, the temperature increase in the recovery container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.

In the twelfth embodiment of the present invention, in the method for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to the eleventh embodiment, a coolant at 20 ° C. to 30 ° C. is supplied to a water cooling jacket.
According to the present embodiment, even if oxygen is contained in the atmosphere in the recovery container and the hydrogen pulverized powder is oxidized during mixing, the temperature rise in the recovery container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.

According to a thirteenth embodiment of the present invention, there is provided a method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to any one of the first and ninth to twelfth embodiments. Is performed by rotating the collection container itself.
According to the present embodiment, when mixing the hydrogen pulverized powder and the lubricant, it is not necessary to transfer to another container, so that it is possible to prevent oxygen from being mixed into the recovery container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.

  An apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to a fourteenth embodiment of the present invention includes a hydrogen storage treatment and heating of a rare earth magnet raw alloy housed in a processing vessel having an opening on the upper surface. One or a plurality of processing chambers for processing and cooling, and a recovery chamber connected to the processing chamber, wherein the recovery chamber has a first gas introduction means for introducing an inert gas, and an oxygen-containing gas. A second gas introduction means for introducing gas, a vacuum exhaust means for discharging the gas in the recovery chamber, a carry-in port for carrying the processing container from the processing chamber into the recovery chamber, and a lower portion of the recovery chamber A discharge port that is disposed, and discharges the hydrogen pulverized powder of the rare earth-based magnet raw material alloy in the processing container carried into the recovery chamber from the processing chamber into the recovery chamber, and the recovery port discharges the recovery port. Rare earth magnet raw material collected in a container An apparatus for producing hydrogen pulverized powder of alloy, wherein the recovery container is provided with a bucket for storing a lubricant in the recovery container and a water cooling jacket for cooling the recovery container on the outer surface of the recovery container. The recovery chamber is provided with a reversing means for turning the processing container upside down and a pressure measuring means for measuring the pressure in the recovery chamber, and is measured by the pressure measuring means after operating the evacuation means. The reversing means is operated based on the pressure information, the processing vessel is turned upside down, and the hydrogen pulverized powder of the rare earth magnet raw material alloy in the processing vessel is discharged into the recovery chamber.

According to the present embodiment, the hydrogen pulverized powder of the rare earth-based magnet raw material alloy accommodated in the processing vessel having an opening on the upper surface is converted into information on the pressure measured by the pressure measuring unit after the vacuum evacuating unit is operated. Based on this, the reversing means is operated, the processing container is turned upside down and discharged into the collection chamber, so that the hydrogen pulverized powder falls without flying in the collection chamber, so that it does not adhere to the wall surface of the collection chamber. Therefore, the hydrogen pulverized powder adhering to the wall surface of the recovery chamber is oxidized when the recovery chamber is opened to the outside air by unloading the processing container, etc. In operation, the low oxygen hydrogen pulverized powder can be mass-produced stably, and the magnetic properties of the rare earth magnet can be improved.
Further, since the processing container is turned upside down by the reversing means, a large amount of hydrogen pulverized powder can be discharged into the collection chamber at a time, so that the time required for collecting the hydrogen pulverized powder can be greatly shortened. Furthermore, since a relatively simple operation of upside down is employed, a large-scale device is not necessary, and the entire collection device can be reduced in size. Moreover, according to the manufacturing apparatus of this invention, the yield of hydrogen pulverized powder can be improved significantly.
In addition, after discharging the hydrogen pulverized powder of the rare earth-based magnet raw material alloy into the collection chamber and before collecting it in the collection container, the first gas introduction means and / or the second gas introduction means in the collection chamber and the inert gas and By introducing an oxygen-containing gas and / or having a predetermined oxygen concentration, the oxygen content of the hydrogen pulverized powder can be controlled within a desired range, and the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder are commonly used. It can be manufactured using a hydrogen pulverizer. Therefore, the manufacturing cost can be reduced, the manufacturing line can be simplified, and the cost required for equipment maintenance can be reduced.
Moreover, since the bucket for accommodating a lubricant in the collection container is disposed, the lubricant can be added to the hydrogen crushed powder in the collection container. Therefore, it is not necessary to release the collection container, and oxygen can be prevented from being mixed into the collection container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
Further, since the water cooling jacket for cooling the recovery container is provided on the outer surface of the recovery container, the hydrogen pulverized powder and the lubricant can be mixed while cooling the recovery container. Therefore, a small amount of oxygen is contained in the atmosphere in the recovery container, such as when adding a powdery lubricant having a relatively low melting point to oxygen hydrogen pulverized powder. Even if it oxidizes, the temperature rise in the collection container due to the heat of reaction can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
Thus, the recovery container is provided with a bucket for storing the lubricant in the recovery container and a water cooling jacket for cooling the recovery container on the outer surface of the recovery container. In any case of oxygen hydrogen pulverized powder, recovery of hydrogen pulverized powder after hydrogen pulverization, addition of lubricant to hydrogen crushed powder, and mixing of hydrogen pulverized powder and lubricant can be performed in a common container.

The fifteenth embodiment of the present invention is an apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to the fourteenth embodiment, comprising oxygen concentration measuring means for measuring the oxygen concentration in the recovery chamber. It is.
According to the present embodiment, the oxygen concentration in the recovery chamber is controlled by adjusting the introduction amount of the inert gas and / or the oxygen-containing gas based on the oxygen concentration measured by the oxygen concentration measuring means, It becomes possible to adjust the oxygen content of the recovered hydrogen pulverized powder to a desired value.

In the sixteenth embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a raw material alloy for rare earth magnets according to the fourteenth or fifteenth embodiment, the pressure measured by the pressure measuring means is 1000 Pa or less. It is.
According to the present embodiment, the hydrogen pulverized powder falls without fluttering in the collection chamber at the time of reversal, and thus can be prevented from adhering to the wall surface of the collection chamber.

According to a seventeenth embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the fourteenth to sixteenth embodiments, the inversion means inverts the processing container upside down. The processing container is further swung with the opening of the container facing downward.
According to the present embodiment, a small amount of hydrogen pulverized powder remaining in the processing container can be completely dropped.

According to an eighteenth embodiment of the present invention, in the apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the fourteenth to seventeenth embodiments, the processing container is a lid that covers the opening of the processing container A lid opening / closing means for removing the body and the lid, wherein the lid opening / closing means engages an engagement piece provided in the lid and an engagement piece provided in the collection chamber, The lid is removed by moving the joint piece upward.
According to the present embodiment, since the engaging pieces are engaged with each other using the transfer operation carried into the collection chamber, the lid opening / closing means opens the lid by simply moving the engaging pieces upward. Can be removed from.

According to a nineteenth embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the eighteenth embodiment, the engagement piece provided on the lid is recovered at the top of the lid. Engagement pieces provided in the chamber are respectively arranged in the upper part of the collection chamber. One engagement piece has a T-shaped cross-sectional shape, and the other engagement piece has a substantially C-shaped cross-sectional shape. It is what.
According to the present embodiment, the engagement pieces can be reliably engaged with each other.

In a twentieth embodiment of the present invention, in the apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any of the fourteenth to nineteenth embodiments, the recovery chamber carries the processing container from the processing chamber. The reversing means reverses the processing container together with the conveyor means.
According to the present embodiment, by inverting the conveyor means together with the processing container, the hydrogen crushed powder discharged from the processing container does not adhere to the conveyor means, and the hydrogen crushed powder is reliably dropped to the lower part of the recovery chamber. be able to.

According to a twenty-first embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a raw material alloy for rare earth magnets according to the twentieth embodiment, the processing container moves on both sides in the processing container transport direction of the conveyor means when reversing. A movement preventing means for preventing the processing container is provided, and a separation preventing means for preventing the processing container from being detached from the conveyor means at the time of reversing is provided on both sides of the conveyor means in the direction orthogonal to the processing container loading direction. The processing container is held at a predetermined position with respect to the conveyor means by the pair of movement prevention means and the pair of separation prevention means.
According to the present embodiment, the processing container can be held at a predetermined position with respect to the conveyor means by the pair of movement prevention means and separation prevention means, and the reversing operation can be reliably performed even in a narrow space. it can.

According to a twenty-second embodiment of the present invention, in the apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to the twenty-first embodiment, the conveyor means is composed of a plurality of rollers, and the movement preventing means is a roller. It is provided so as to be able to appear on the processing container side from between.
According to the present embodiment, the apparatus can be reduced in size to use the gap between the rollers, and the positional relationship with the rollers can be easily maintained, so that the processing container can be reliably held.

According to a twenty-third embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the twenty-first or twenty-second embodiment, the separation preventing means has an L-shaped cross-sectional shape, It arrange | positions so that it may be located in the upper part of the collar part provided in the outer periphery of the opening part vicinity.
According to the present embodiment, by forming the collar part, the collar part and the separation preventing means can be made to correspond to each other by the transport operation, and the processing container can be held at a predetermined position.

According to a twenty-fourth embodiment of the present invention, in the apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of the fourteenth to twenty-third embodiments, the outlet has a valve, The annular expansion member disposed on the inner peripheral surface of the cylindrical member, and a disk member having the radial direction of the cylindrical member as a rotation axis.
According to the present embodiment, it is possible to eliminate the influence due to the adhesion of the hydrogen pulverized powder and maintain the sealing property.

According to a twenty-fifth embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the fourteenth embodiment, a lubricant is added to the recovery container by inverting the bucket in the recovery container. To be discharged.
According to the present embodiment, the recovery container is not released, and oxygen can be prevented from being mixed into the recovery container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.

According to a twenty-sixth embodiment of the present invention, in the apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to the fourteenth embodiment, a coolant at 20 ° C. to 30 ° C. is supplied to a water cooling jacket on the outer surface of the recovery container. Is.
According to the present embodiment, even if a large amount of oxygen is contained in the atmosphere in the collection container and the hydrogen pulverized powder is oxidized during mixing, the temperature rise in the collection container can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.

Example 1
Hereinafter, a method and apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to an embodiment of the present invention will be described.
FIG. 1 is a block diagram illustrating a method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to an embodiment of the present invention. As shown in the figure, the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy of this example is a hydrogen pulverization process comprising a hydrogen storage process, a heating process, and a cooling process, a hydrogen pulverized powder recovery process, It has a lubricant addition step of adding a lubricant to the pulverized powder and a mixing step of mixing the hydrogen pulverized powder and the lubricant.
The production method of the present embodiment, in the recovery step in the hydrogen pulverization step, recovers the hydrogen pulverized powder after decompressing the recovery chamber, thereby preventing the hydrogen pulverized powder from adhering to the wall surface of the recovery chamber. The pulverized powder can be mass-produced. However, in order to produce a low-oxygen magnet having excellent magnetic properties, it is described in Patent Documents 1 and 2 in order to prevent oxidation of finely pulverized powder having a small particle size and being easily oxidized, particularly after each step of hydrogen pulverization. As a result, new devices and processes must be employed, which increases manufacturing costs. For this reason, depending on the use of the rare earth magnet, as described in Patent Document 4, jet mill pulverization is performed in an inert gas containing a specific amount of oxygen to form an oxide film on the surface of the finely pulverized powder. By stabilizing the pulverized powder, it is possible to perform press molding in the atmosphere, and there is also a demand for a normal oxygen magnet with improved press molding efficiency and reduced manufacturing costs. However, when low-oxygen hydrogen pulverized powder for low-oxygen magnets is normally used in the production of oxygen magnets, there is a limit to the increase in oxygen content even if jet milling is performed in an inert gas containing a specific amount of oxygen. Yes, the formation of oxide film on the surface of finely pulverized powder is not sufficient, and it cannot be completely stabilized, and problems such as ignition of finely pulverized powder due to rapid oxidation during press molding in the air occur. To do. That is, when manufacturing a normal oxygen magnet, it is necessary to prepare a normal oxygen hydrogen pulverized powder for a normal oxygen magnet containing a specific amount of oxygen in advance. Therefore, it is necessary to control the oxygen content within a specific range at the stage of hydrogen pulverized powder.

  In addition, the following reasons can be considered that there is a limit in the increase in oxygen content even if it pulverizes by the jet mill in the inert gas containing a specific amount of oxygen. In fine pulverization by a jet mill, it is common to classify and remove ultrafine powder having a small particle diameter by a classifier such as a classifying rotor or a cyclone classifier. The ultrafine powder is very easy to oxidize because of its large specific surface area, and the ultrafine powder contains much R in the R-T-B magnet so that the degree of oxidation is even more intense. In particular, the raw material alloy produced by the strip casting method has a refined structure and the fine R-rich phase is uniformly dispersed, so that the R-rich phase is likely to appear on the surface of the hydrogen pulverized powder particles. The R-rich phase is oxidized and removed as ultrafine powder by a classifier. Since the ultrafine powder is preferentially oxidized and consumes oxygen in the inert gas, it is easy to greatly increase the oxygen content of the finely pulverized powder obtained after classifying and removing the ultrafine powder. is not.

Therefore, in the production method according to the present embodiment, in the recovery process for recovering the hydrogen pulverized powder after the hydrogen storage process, the heating process, and the cooling process, the hydrogen pulverized powder is discharged into the decompressed recovery chamber and then inactivated in the recovery chamber. A gas and / or an oxygen-containing gas is introduced, and the oxygen content of the hydrogen pulverized powder is adjusted with a predetermined pressure and a predetermined oxygen concentration in the recovery chamber. Thereby, the oxygen content of hydrogen ground powder can be adjusted to a desired value. Therefore, according to the recovery method of the present embodiment, not only low oxygen hydrogen pulverized powder suitable for low oxygen magnets but also normal oxygen hydrogen pulverized powder suitable for normal oxygen magnets can be obtained.
As described above, according to the manufacturing method according to the present embodiment, the oxygen content of the hydrogen pulverized powder is adjusted by simultaneously introducing the oxygen-containing gas and / or the inert gas into the recovery chamber in the recovery step, and its use Can be recovered as having an oxygen content corresponding to. Therefore, the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder can be produced using a common hydrogen pulverizing apparatus.
Further, in the manufacturing method according to the present embodiment, a lubricant is added to the hydrogen crushed powder in a collection container containing the hydrogen crushed powder collected in the collecting step. Thereby, it is not necessary to release the collection container, and oxygen can be prevented from being mixed into the collection container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
Moreover, in the manufacturing method according to the present embodiment, the recovery container containing the hydrogen pulverized powder to which the lubricant is added is mixed while being cooled. This allows oxygen to be contained in the atmosphere in the recovery container, such as when adding a powdery lubricant having a relatively low melting point to the oxygen hydrogen pulverized powder, and the hydrogen pulverized powder gradually oxidizes during mixing. The temperature rise in the collection container can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
In this way, the lubricant is added to the hydrogen pulverized powder in the recovery container, and the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. In this case, the hydrogen pulverized powder recovered after hydrogen pulverization, the addition of a lubricant to the hydrogen pulverized powder, and the mixing of the hydrogen pulverized powder and the lubricant can be performed in a common container.

FIG. 2 is a schematic diagram showing a schematic configuration of an apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to the present embodiment. As shown in the figure, the manufacturing apparatus according to the present embodiment includes a hydrogen storage chamber 10, a heating chamber 20, a cooling chamber 30, a recovery chamber 40, and a recovery container 1. The hydrogen pulverized powder obtained by the manufacturing apparatus according to the present embodiment is recovered in the recovery container 1 and a lubricant is added in the recovery container 1. Next, the recovery container 1 is detached from the recovery chamber 40, the recovery container 1 is fixed to the mixing device 70, and the recovery container 1 itself is rotated by the mixing device 70 while cooling the recovery container 1, whereby hydrogen pulverized powder and lubricant Mix. When mixing is completed, the collection container 1 is removed from the mixing device 70, and after the collection container 1 is connected to the raw material tank of the jet mill device 80, hydrogen pulverized powder mixed with a lubricant is supplied to the jet mill device 80. Grind finely. The obtained finely pulverized powder is then molded in a dry or wet process, and a rare earth magnet is manufactured through each step of sintering and heat treatment.
In the above description, the lubricant is added before the collection container 1 is detached from the collection chamber 40. However, the lubricant may be added in a state where the collection container 1 is detached from the collection chamber 40.

FIG. 3 is a front view schematically showing the structure of the collection container 1 and the mixing device 70 of the present embodiment. As shown in the figure, the recovery container 1 is provided with a water cooling jacket 1 b for cooling the recovery container 1 on the outer surface of the recovery container 1. The water cooling jacket 1b is provided with a refrigerant inlet 1a and a refrigerant outlet 1c. Below, the cooling method of the collection container 1 is demonstrated.
The mixing device 70 includes a recovery container fixing part 71 that fixes the recovery container 1, a main body 72, a connection part 73, a refrigerant path 74, and a rotary joint 75.
The collection container fixing unit 71 accommodates and fixes the collection container 1, and the other end is rotatable about the upper one end as an axis as shown by a broken line. Thereby, the collection container 1 can be accommodated easily. The collection container fixing part 71 is connected to the main body 72 via a connection part 73 and rotates around the connection part 73 as shown by a two-dot chain line in the drawing. Note that the rotation direction of the collection container fixing portion 71 may be opposite to the above.

The recovery container 1 is fixed to the recovery container fixing part 71 of the mixing device 70, and the refrigerant inlet 1 a and the refrigerant outlet 1 c of the recovery container 1 are connected to the refrigerant path 74 of the mixing device 70. The refrigerant is injected into the water cooling jacket 1b from the refrigerant path 74 of the mixing device 70 through the refrigerant inlet 74a as shown by arrows in the drawing, and discharged from the refrigerant outlet 1c. Thereby, the temperature of the water in the water cooling jacket 1b can be maintained below a predetermined temperature. For this reason, even if oxygen is contained in the atmosphere in the recovery container 1 and the hydrogen pulverized powder is gradually oxidized by the oxygen during mixing, the temperature rise in the recovery container 1 due to the reaction heat can be prevented. . Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
In addition, in the above, although the case where oxygen was contained in the atmosphere in the collection container 1 was described, oxygen is contained in the atmosphere in the collection container 1 when manufacturing low oxygen hydrogen pulverized powder, for example. Even if not, the temperature in the collection container 1 rises due to friction between the hydrogen pulverized powders during mixing. Even in these cases, the same effects as described above can be obtained by mixing while cooling using the collection container 1 according to the present embodiment.
In addition, when producing oxygen hydrogen pulverized powder, the oxygen content is adjusted when recovering hydrogen pulverized powder from the recovery chamber to the recovery container 1 even if the recovery container 1 has low oxygen (20 ppm or less). Oxygen-containing gas introduced for this purpose may be mixed in the recovery container 1 with a small amount of hydrogen pulverized powder. Even in these cases, the same effects as described above can be obtained by mixing while cooling using the collection container 1 according to the present embodiment.
Furthermore, in the manufacturing apparatus according to the present embodiment, the processing container 1 has a structure that can be attached to and detached from the recovery chamber. Due to the structure of the attaching / detaching portion, it is difficult to depressurize the inside of the processing container 1 by a vacuum exhaust means. Accordingly, the oxygen concentration is lowered in the processing container 1 by the flow of the inert gas. For example, the oxygen concentration does not decrease to a predetermined value (20 ppm or less) due to some trouble, or the oxygen concentration measuring means is broken. It is also conceivable that a small amount of oxygen is mixed into the recovery chamber 1 due to the above. Even if such a sudden trouble occurs, according to the manufacturing apparatus according to the present embodiment, the lubricant does not stick to the inner wall of the collection container 1 and the lubricant does not peel off during the next mixing. The collection container 1 is not affected by trouble.
In FIG. 3, for convenience of explanation, the flow of water near the center of the recovery container 1 is indicated by an arrow. However, the water cooling jacket 1b of the present embodiment is disposed in the entire recovery container 1, and the front of FIG. Cooling water also flows on the side and back surfaces. However, the water cooling jacket 1b does not necessarily have to be disposed in the entire collection container 1.
In the present embodiment, couplers (connectors) are provided at the refrigerant inlet 1a, the refrigerant outlet 1c, and the ends of the refrigerant path 74 so that they can be easily detached. Further, since the rotary joint 75 is provided in the refrigerant path 74, the refrigerant path 74 can be rotated according to the rotation of the collection container fixing portion 71.

FIG. 4 is a partially broken cross-sectional view for explaining the configuration inside the collection container 1. As shown in the figure, the collection container 1 is provided with a bucket 1 d for containing the lubricant in the collection container 1. Before the hydrogen pulverized powder is collected in the recovery container 1, the lubricant can be added to the hydrogen pulverized powder in the recovery container 1 by storing the lubricant in the bucket 1d in advance. Therefore, it is not necessary to release the collection container 1 and oxygen can be prevented from being mixed into the collection container 1. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced. Before the hydrogen pulverized powder is collected in the collection container 1, it is possible to put a lubricant into the bottom of the collection container 1, but when the hydrogen crushed powder is collected, The lubricant may stick to the bottom of the collection container 1 with the weight of or may adhere to only a part of the hydrogen pulverized powder and may not be sufficiently mixed in the subsequent mixing step. Therefore, it is preferable to store the lubricant in the bucket 1d.
The lubricant can be easily discharged from the bucket 1d by reversing the bucket 1d with an operation rod (not shown).
Further, as indicated by a broken line in FIG. 4, the lubricant can be more easily discharged from the bucket 1d by making the inner surface shape of the bucket 1d hemispherical. Further, when the hydrogen pulverized powder falls from the collection chamber into the collection container 1, a part of the hydrogen pulverized powder enters the bucket 1d, and the lubricant in the bucket 1d is pushed out little by little and falls into the collection container 1. Therefore, the lubricant can be added more efficiently.

FIG. 5 is a view schematically showing a method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy and subsequent steps according to this example. As shown in the figure, the production method of the present invention includes a hydrogen pulverization step, a hydrogen pulverized powder recovery step, a lubricant addition step for adding a lubricant to the hydrogen pulverized powder, and a mixing step for mixing the hydrogen pulverized powder and a lubricant. have. The hydrogen pulverized powder in which the lubricant is mixed in the mixing step becomes a finely pulverized powder through the fine pulverizing step.
The production method of the present embodiment, in the recovery step, recovers the hydrogen pulverized powder after decompressing the recovery chamber, thereby preventing the hydrogen pulverized powder from remaining on the wall surface of the recovery chamber. Can be mass-produced. However, as described above, in order to produce a low-oxygen magnet having excellent magnetic properties, each step after hydrogen pulverization, particularly in order to prevent oxidation of finely pulverized powder having a small particle size and being easily oxidized, is disclosed in Patent Document 1. As described in (2) and (2), a new apparatus and process must be employed, which increases the manufacturing cost. For this reason, depending on the use of the rare earth magnet, as described in Patent Document 4, jet mill pulverization is performed in an inert gas containing a specific amount of oxygen to form an oxide film on the surface of the finely pulverized powder. By stabilizing the pulverized powder, it is possible to perform press molding in the atmosphere, and there is also a demand for a normal oxygen magnet with improved press molding efficiency and reduced manufacturing costs. However, when low-oxygen hydrogen pulverized powder for low-oxygen magnets is normally used in the production of oxygen magnets, there is a limit to the increase in oxygen content even if jet milling is performed in an inert gas containing a specific amount of oxygen. Yes, the formation of oxide film on the surface of finely pulverized powder is not sufficient, and it cannot be completely stabilized, and problems such as ignition of finely pulverized powder due to rapid oxidation during press molding in the air occur. To do. That is, when manufacturing a normal oxygen magnet, it is necessary to prepare a normal oxygen hydrogen pulverized powder for a normal oxygen magnet containing a specific amount of oxygen in advance. Therefore, it is necessary to control the oxygen content within a specific range at the stage of hydrogen pulverized powder.

Therefore, the method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to the present example is a recovery chamber that is decompressed in a recovery step of recovering the rare earth magnet raw material alloy that has undergone the hydrogen storage process, heating process, and cooling process. After the rare earth magnet raw material alloy is discharged, an inert gas and / or oxygen-containing gas is introduced into the recovery chamber, and the oxygen content of the hydrogen pulverized powder is adjusted with the recovery chamber at a predetermined pressure and a predetermined oxygen concentration. Thereby, the oxygen content of hydrogen ground powder can be adjusted to a desired value. Therefore, according to the manufacturing method of the present embodiment, not only low oxygen hydrogen pulverized powder suitable for low oxygen magnets but also normal oxygen hydrogen pulverized powder suitable for normal oxygen magnets can be obtained.
Thus, according to the manufacturing method of the present embodiment, the low oxygen hydrogen pulverized powder and the normal oxygen hydrogen pulverized powder can be manufactured using a common hydrogen pulverizer. Therefore, the manufacturing cost can be reduced, the manufacturing line can be simplified, and the cost required for equipment maintenance can be reduced.
In addition, since the lubricant is added to the hydrogen pulverized powder in the recovery container in the lubricant addition step, it is not necessary to open the recovery container, and oxygen can be prevented from being mixed into the recovery container. Therefore, the hydrogen pulverized powder after hydrogen pulverization can be recovered, the lubricant added to the hydrogen pulverized powder, and the hydrogen pulverized powder and the lubricant can be mixed while maintaining an oxygen-free state. Less low oxygen hydrogen pulverized powder can be produced.
In addition, in the mixing process, the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container, so the recovery container is usually used when adding a solid or powdered lubricant having a relatively low melting point to the oxygen hydrogen pulverized powder. Even if oxygen is contained in the inside atmosphere and the hydrogen pulverized powder is gradually oxidized during the mixing, the temperature rise in the recovery container due to the reaction heat can be prevented. Therefore, a predetermined amount of the lubricant can be uniformly mixed with the hydrogen pulverized powder without the lubricant sticking to the inner wall of the collection container and the lubricant does not peel off during the next mixing.
In this way, the lubricant is added to the hydrogen pulverized powder in the recovery container, and the hydrogen pulverized powder and the lubricant are mixed while cooling the recovery container. In this case, the hydrogen pulverized powder recovered after hydrogen pulverization, the addition of a lubricant to the hydrogen pulverized powder, and the mixing of the hydrogen pulverized powder and the lubricant can be performed in a common container.

FIG. 6 is a schematic configuration diagram of an apparatus for producing hydrogen pulverized powder of a rare earth magnet raw material alloy according to this embodiment.
As shown in FIG. 6, the hydrogen pulverizing apparatus for a rare earth magnet raw material alloy according to the present embodiment includes a hydrogen storage chamber 10 for storing hydrogen in the rare earth magnet raw material alloy, and a rare earth magnet pulverized by hydrogen storage. A heating chamber 20 that dehydrogenates the raw material alloy by heating, a cooling chamber 30 that cools the heated rare earth magnet raw material alloy, and a hydrogen pulverized powder of the cooled rare earth magnet raw material alloy is recovered in the recovery container 1. And a recovery chamber 40.
The hydrogen storage chamber 10 has a shut-off door 11 at the entrance to the front chamber and a shut-off door 21 at the exit to the heating chamber 20 so as to keep the room sealed. The hydrogen storage chamber 10 includes an inert gas introduction unit 12 that introduces an inert gas, a vacuum exhaust unit 13 that exhausts indoor gas, a hydrogen introduction unit 14 that introduces hydrogen gas, and a conveyor that conveys the processing vessel 50. Means 15 are provided.
The heating chamber 20 has a shut-off door 21 at the carry-in port from the hydrogen storage chamber 10 and a shut-off door 31 at the carry-out port to the cooling chamber 30 so as to keep the inside of the room sealed. The heating chamber 20 includes an inert gas introduction unit 22 for introducing an inert gas, a vacuum exhaust unit 23 for discharging the indoor gas, a heating unit 24 for heating the room, and a conveyor unit 25 for conveying the processing container 50. I have.
The cooling chamber 30 has a shut-off door 31 at the entrance to the heating chamber 20 and a shut-off door 41 at the exit to the recovery chamber 40 so as to keep the room sealed. The cooling chamber 30 includes an inert gas introduction means 32 for introducing an inert gas, a vacuum exhaust means 33 for discharging the indoor gas, a cooling means 34 for cooling the room, and a conveyor means 35 for conveying the processing container 50. I have.
The recovery chamber 40 has a shut-off door 41 at the carry-in port from the cooling chamber 30 and a shut-off door 2 at the carry-out port to the outside of the furnace, and is configured to keep the room sealed. The recovery chamber 40 includes a first gas introduction unit 42a that introduces an inert gas, a second gas introduction unit 42b that introduces an oxygen-containing gas, a vacuum exhaust unit 43 that exhausts indoor gas, and a processing vessel 50. Is provided with a reversing means 44 for turning the processing container 50 up and down and a conveyor means 45 for conveying the processing container 50. In addition, a valve 60 is provided below the collection chamber 40, and the collection container 1 is connected via the valve 60. The collection container 1 is provided with a valve (not shown) for sealing the container.
The processing vessel 50 is transferred to the hydrogen storage chamber 10, the heating chamber 20, the cooling chamber 30, and the recovery chamber 40 in a state where the rare earth magnet raw material alloy is accommodated.

  In the present invention, as described above, the hydrogen occlusion process, the heating process, and the cooling process are performed in one room in addition to the so-called continuous furnace type hydrogen pulverization apparatus in which the hydrogen storage chamber, the heating chamber, and the cooling chamber are independent from each other. A so-called batch furnace (independent furnace) type hydrogen pulverizer can be used. In addition, the hydrogen storage chamber / heating chamber and cooling chamber, the hydrogen storage chamber / heating chamber / cooling chamber, etc., and a plurality of heating chambers and cooling chambers are provided to improve the processing capacity. Alternatively, a hydrogen pulverizer configured as a second heating chamber, a first cooling chamber, or a second cooling chamber may be used. Furthermore, a hydrogen pulverization apparatus having a configuration in which a preparation chamber and a spare chamber are installed in front of the hydrogen storage chamber may be used. That is, all known hydrogen pulverizers can be used for the portions other than the recovery chamber.

Further, the first gas introduction means 42a for introducing the inert gas and the second gas introduction means 42b for introducing the oxygen-containing gas do not need to be separately connected to the recovery chamber 40. For example, the recovery chamber 40 The first gas introducing means 42a and the second gas introducing means 42b may be combined with each other and connected to the recovery chamber 40 as one gas introducing means before being connected to. In this case, when the inert gas and the oxygen-containing gas are introduced simultaneously, a mixing device for mixing the oxygen-containing gas and the inert gas may be provided before introducing the gas into the recovery chamber 40.
Further, when air is used as the oxygen-containing gas, it is preferable to provide a dry air generator at the front stage of the second gas introduction means 42b. By providing a dry air generator, the influence of moisture contained in the air on the oxidation of hydrogen pulverized powder can be suppressed, and the oxygen content of the hydrogen pulverized powder is accurately adjusted by a predetermined value. It becomes possible. As the dry air generator, a known generator such as a refrigeration type or an adsorption type can be used. The dry air generated by the dry air generator is preferably at atmospheric dew point of −10 ° C. or lower.

The raw material alloy for rare earth magnets to be treated by this apparatus is preferably an R—T—B magnet raw material alloy, desirably an R—Fe (Co) —BM system.
R is selected from at least one of Nd, Pr, Dy, and Tb. However, it is desirable that R always contains either Nd or Pr. More preferably, a combination of rare earth elements represented by Nd-Dy, Nd-Tb, Nd-Pr-Dy, or Nd-Pr-Tb is used.
Of R, Dy and Tb are particularly effective in improving the coercive force. In addition to the above elements, a small amount of other rare earth elements such as Ce and La may be contained, and misch metal or didymium can also be used. Further, R may not be a pure element, and may contain impurities that are unavoidable in the manufacturing process within a commercially available range. A conventionally known content can be adopted as the content, and for example, a range of 25% by mass to 35% by mass is a preferable range. If the amount is less than 25% by mass, high magnetic properties, particularly high coercive force cannot be obtained, and if it exceeds 35% by mass, the residual magnetic flux density decreases.
T necessarily contains Fe, and 50% or less can be substituted with Co. Co is effective in improving temperature characteristics and corrosion resistance, and is usually used in a combination of 10 mass% or less of Co and the balance Fe. The content of T occupies the remainder of R and B or R, B and M.
The content of B may be a known content, and for example, 0.9 mass% to 1.2 mass% is a preferable range. If it is less than 0.9% by mass, a high coercive force cannot be obtained, and if it exceeds 1.2% by mass, the residual magnetic flux density decreases, which is not preferable. A part of B can be replaced with C. C substitution is effective because it can improve the corrosion resistance of the magnet. The content in the case of B + C is preferably set within the above range of B concentration by converting the number of C substitution atoms by the number of B atoms.
In addition to the above elements, an M element can be added to improve the coercive force. The element M is at least one of Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Zr, Nb, Mo, In, Sn, Hf, Ta, and W. The addition amount is preferably 2% by mass or less. This is because the residual magnetic flux density decreases when the content exceeds 5 mass%.
Inevitable impurities can also be tolerated. For example, Mn, Cr mixed from Fe, Al, Si, Cu mixed from Fe-B (ferroboron), and the like.

The raw material alloy for rare earth magnets carried into the apparatus is manufactured by a melting method. Dissolve the metal that has been adjusted in advance to the final required composition, put it into the mold, ingot casting method, or bring the molten metal into contact with a single roll, twin roll, rotating disk, rotating cylindrical mold, etc. Manufactured by a rapid cooling method typified by a strip casting method or a centrifugal casting method for producing a solidified alloy thinner than an alloy made by an ingot method. The rare earth magnet raw material alloy according to the present embodiment can be applied to a material manufactured by either an ingot method or a rapid cooling method, but is preferably manufactured by a rapid cooling method.
The thickness of the rare earth magnet raw material alloy (quenched alloy) produced by the rapid cooling method is in the range of 0.03 mm or more and 10 mm or less, and has a flake shape. The molten alloy begins to solidify from the contact surface (roll contact surface) of the cooling roll, and crystals grow in a columnar shape from the roll contact surface in the thickness direction. The quenched alloy is cooled in a short time compared to an alloy (ingot alloy) produced by a conventional ingot casting method (die casting method), so that the structure is refined and the crystal grain size is small. Further, since the area of the grain boundary is wide and the R-rich phase spreads widely within the grain boundary, the dispersibility of the R-rich phase is excellent. For this reason, it is easy to break at the grain boundary by the hydrogen pulverization method. By subjecting the quenched alloy to hydrogen pulverization, the average size of the hydrogen pulverized powder (coarse pulverized powder) can be set to, for example, 1.0 mm or less.

The hydrogen crushing apparatus according to the present embodiment shows a configuration in which the hydrogen storage chamber 10, the heating chamber 20, the cooling chamber 30, and the recovery chamber 40 are connected to each other. A plurality of cooling chambers 30 may be provided.
The processing container 50 has an opening on the upper surface, and a lid 51 is provided in the opening. Here, the lid 51 does not seal the opening, but has a gap through which hydrogen gas, inert gas, and the like can enter and exit. That is, the opening of the processing container 50 is covered with the lid. The processing vessel 50 is suitably made of stainless steel that is heat resistant and relatively easy to process. What is necessary is just to determine a volume and board thickness suitably according to the quantity processed at once and the dimension of a hydrogen pulverizer. The processing container 50 does not stick to the shape as long as the upper part is open, but generally has a box shape. In order to improve the efficiency of hydrogen occlusion, heating, and cooling, it is also one of preferable configurations to arrange a plurality of box-shaped containers at a fixed interval on one pedestal. By the way, in this embodiment, a processing container is used in which box-shaped containers are arranged on one pedestal at a predetermined interval of 4 rows × 2 rows. Further, it is desirable that the processing container 50 includes a pipe penetrating the inside. Since the raw material alloy is charged and deposited in the processing vessel 50, the temperature change inside the processing vessel 50 due to heating or cooling is slow, and the dehydrogenation or cooling after dehydrogenation is not sufficient, and the finally obtained magnet Therefore, by passing an inert gas for heating or cooling through the pipe passing through the inside, there is a difference in temperature change between the raw material alloy on the surface of the processing vessel 50 and the internal raw material alloy. Reduced and quality stabilized. The pipes can be further improved in temperature change of the raw material alloy by combining pipes having different diameters or selecting an arrangement place and an arrangement interval.
The processing container 50 is transferred to the hydrogen storage chamber 10, the heating chamber 20, and the cooling chamber 30 with the opening covered with the lid 51.

The operation of the hydrogen pulverizer according to this embodiment will be described below with reference to FIG.
The processing container 50 carried into the hydrogen storage chamber 10 contains a flaky rare earth magnet raw material alloy manufactured by, for example, a rapid cooling method.
The shut-off door 11 of the hydrogen storage chamber 10 is opened and the processing container 50 is carried into the hydrogen storage chamber 10. After carrying in, the shut-off door 11 is closed, and the vacuum exhaust means 13 is operated to evacuate the hydrogen storage chamber 10.
After the inside of the hydrogen storage chamber 10 is evacuated and the operation of the evacuation unit 13 is completed, the hydrogen introduction unit 14 is operated to introduce hydrogen gas into the hydrogen storage chamber 10. By introducing hydrogen gas, the inside of the hydrogen storage chamber 10 is brought to a pressure of 0.1 to 0.18 MPa, and hydrogen is stored in the rare earth-based magnet raw material alloy in the processing vessel 50 to perform the hydrogen storage step.
After a predetermined time has elapsed (after the completion of hydrogen storage), the operation of the hydrogen introduction unit 14 is terminated to stop the introduction of hydrogen gas, and the hydrogen gas in the hydrogen storage chamber 10 is evacuated by operating the vacuum evacuation unit 13. To do. As a result, the hydrogen occlusion process ends, and the process proceeds to the next heating process. At this time, the rare earth-based magnet raw material alloy absorbs hydrogen and becomes brittle and pulverized to form hydrogen pulverized powder (coarse pulverized powder).

Since the hydrogenation reaction for storing hydrogen is an exothermic reaction, the temperature of the raw material alloy increases with the storage of hydrogen. Usually, when this exothermic reaction is finished and the temperature of the raw material alloy is lowered and stabilized, it is considered that the hydrogen occlusion is finished and the process proceeds to the next heating step. However, it takes a long time for the temperature to decrease and stabilize, and when the raw material alloy whose temperature has decreased is transferred to the heating chamber, the temperature of the heating chamber decreases and it takes time to reach a predetermined temperature. It will be.
Therefore, a method for storing the hydrogen in a state of maintaining a high temperature without reducing the temperature by using the temperature increase of the raw material alloy due to the exothermic reaction during the hydrogen storage is configured so that the hydrogen storage chamber can be heated. Adopting is one of the preferred means. By performing hydrogen occlusion while maintaining a high temperature, hydrogen occlusion is performed mainly in the R-rich phase at the grain boundary, so that the time required for the hydrogen occlusion process and the amount of introduced hydrogen are reduced while sufficiently progressing the embrittlement of the raw material alloy. be able to. Moreover, since it can also prevent the temperature fall of a heating chamber if it transfers to the subsequent heating process, maintaining a high temperature holding state, the time of the heating process in a heating chamber can be shortened and the power consumption required for a heating can be reduced.

Next, when moving to the heating step, the processing container 50 is transferred from the hydrogen storage chamber 10 to the heating chamber 20, and the inside of the heating chamber 20 is evacuated in advance by the evacuation means 23 during the transfer.
The processing container 50 is carried into the heating chamber 20 from the hydrogen storage chamber 10 by opening the blocking door 21 and driving the conveyor means 15 and the conveyor means 25. After carrying in, the shut-off door 21 is closed, and the inside of the heating chamber 20 is further evacuated by the vacuum exhaust means 23 and heated by the heating means 24. The inside of the heating chamber 20 is maintained at a temperature of 500 to 600 ° C. by the heating unit 24 and maintained at a pressure of about 1 Pa by the vacuum exhaust unit 23. Thereby, the hydrogen pulverized powder is dehydrogenated. In the heating process of the hydrogen pulverized powder, the inside of the heating chamber 20 is evacuated as described above. At the same time as the evacuation, an inert gas (for example, argon gas) is introduced to be in a flowing state at a predetermined pressure. As a result, the rate of temperature increase of the raw material alloy can be increased, and the time required for the heating process can be shortened.

After the hydrogen pulverized powder has been sufficiently dehydrogenated, an inert gas (for example, argon gas) is introduced into the heating chamber 20 by operating the inert gas introducing means 22, and the atmosphere in the cooling chamber 30 is introduced. After approaching, the operation of the inert gas introduction means 22 is terminated.
The processing container 50 in the heating chamber 20 is carried into the cooling chamber 30 from the heating chamber 20 by opening the blocking door 31 and driving the conveyor means 25 and the conveyor means 35. After carrying in, the blocking door 31 is closed, and the inside of the cooling chamber 30 is cooled by the cooling means 34.
Cooling is performed by cooling with a fan, cooling with cooling water circulation in the cooling chamber, or a combination thereof.
The processing container 50 in the cooling chamber 30 is carried into the recovery chamber 40 from the cooling chamber 30 by opening the blocking door 41 and driving the conveyor means 35 and the conveyor means 45.
In carrying into the recovery chamber 40, an inert gas (argon gas) is introduced into the recovery chamber 40 by operating the first gas introduction means 42 a, and the first atmosphere is brought close to the atmosphere in the cooling chamber 30. The operation of the gas introducing means 42a is terminated.
When producing low oxygen hydrogen pulverized powder, the inert gas is introduced by operating the first gas introducing means 42a as described above, and when normally producing oxygen hydrogen pulverized powder, the above inert gas is used. Instead of gas, an oxygen-containing gas may be introduced by the second gas introduction means 42b, or an inert gas and an oxygen-containing gas may be introduced simultaneously by the first gas introduction means 42a and the second gas introduction means 42b. it can. However, in this case, the oxygen-containing gas also flows into the cooling chamber 30, which is not preferable in terms of managing the oxygen concentration in the cooling chamber 30. Therefore, it is preferable to introduce the oxygen-containing gas after discharging the hydrogen pulverized powder into the recovery chamber 40, and it is preferable to use an inert gas here.
When the processing container 50 is carried into the collection chamber 40, the blocking door 41 is closed, and the inside of the collection chamber 40 is evacuated by operating the evacuation means 43. In a state where the inside of the collection chamber 40 is evacuated to a pressure of 1000 Pa to 1 Pa, preferably 5 Pa to 1 Pa, the lid 51 is removed and the reversing means 44 is operated to remove the hydrogen crushed powder in the processing container 50. Drop on the inner bottom and discharge. The reversing means 44 is a preferable means for discharging the hydrogen pulverized powder in the processing container 50 into the recovery chamber 40. One of the main features of the recovery method of the present invention is that That is, when the hydrogen pulverized powder is discharged into the collection chamber 40, the inside of the collection chamber 40 is decompressed. Therefore, as long as the inside of the collection chamber 40 is depressurized, discharge means other than the reversing means 44 may be used.

In the above, the reason why the pressure in the recovery chamber 40 is set to 1000 Pa to 1 Pa, preferably 5 Pa to 1 Pa is as follows.
After the recovery process is completed, the collection chamber 40 is evacuated after the emptied processing container 50 is taken out from the blocking door 2 and then the blocking door 2 is closed, until the next processing container 50 comes from the cooling chamber. Has been continued.
Then, since the pressure is restored by the inert gas (argon gas) to bring it closer to the cooling chamber atmosphere immediately before the next processing container 50 is carried in, the amount of oxygen in the recovery chamber 40 is sufficiently reduced (for example, 20 ppm or less), from the viewpoint of preventing oxidation of the hydrogen pulverized powder, it is almost unnecessary to consider the amount of oxygen. Therefore, the pressure of 1000 Pa to 1 Pa defines the condition that the hydrogen pulverized powder does not fly in the recovery chamber. On the other hand, if the cycle speed of the hydrogen pulverizer is high, or if the vacuum chamber is not sufficiently evacuated until the next processing container 50 comes from the cooling chamber due to inspection or maintenance in the recovery chamber 40, the recovery chamber In order to sufficiently reduce the amount of oxygen in 40 and preferably to make the amount of oxygen 20 ppm or less, the pressure in the recovery chamber 40 is preferably 5 Pa to 1 Pa. That is, the pressure of 5 Pa to 1 Pa defines the conditions for reducing the amount of oxygen in the recovery chamber 40 to 20 ppm or less. Naturally, since 5 Pa is a higher vacuum than 1000 Pa, the hydrogen pulverized powder does not fly in the recovery chamber. Thus, the pressure in the collection chamber 40 is usually sufficient at 1000 Pa or less, and more preferably 5 Pa or less.
In the present invention, the degree of vacuum of 1 Pa or less is not necessarily required in order to prevent oxidation of hydrogen pulverized powder and dance of hydrogen pulverized powder in the recovery chamber 40, but the present invention can be implemented even if it is 1 Pa or less.
After dropping the hydrogen pulverized powder into the recovery chamber 40, the operation of the vacuum exhaust means 43 is terminated, and the first gas introduction means 42a and / or the second gas introduction means 42b are operated in the recovery chamber 40. After introducing the inert gas and / or the oxygen-containing gas to a predetermined pressure, the operation of the first gas introduction means 42a and / or the second gas introduction means 42b is terminated.
Note that a valve (not shown) provided in the recovery container 1 is opened in the recovery container 1, and the air in the recovery container 1 is previously replaced with an inert gas so that the oxygen concentration is 20 ppm or less. is doing. In addition, by introducing an inert gas (argon gas) into the recovery chamber 40, the predetermined pressure in the recovery chamber 40 is the same as the pressure in the recovery container 1. In this state, the valve 60 is opened to collect the hydrogen pulverized powder in the collection container 1.
When the recovery of the hydrogen pulverized powder into the recovery container 1 is completed, the valve 60 and a valve (not shown) provided in the recovery container 1 are closed, and the recovery container 1 is separated from the recovery chamber 40. Thereafter, the blocking door 2 is opened and the processing container 50 is transferred out of the collection chamber 40.
At this time, in order to maintain the oxygen concentration of the hydrogen pulverized powder adjusted in the recovery chamber 40 until the next pulverization step, an inert gas is introduced into the recovery container 1 in advance as described above. It is preferable that the oxygen concentration be 20 ppm or less. On the other hand, when it is desired to further increase the oxygen concentration of the hydrogen pulverized powder adjusted in the recovery chamber 40, the oxygen concentration exceeds 20 ppm by introducing an inert gas and / or an oxygen-containing gas into the recovery container 1. You may adjust it.

In the present embodiment, the recovery process is performed in a recovery chamber 40 connected to one or a plurality of processing chambers that perform a hydrogen storage process, a heating process, and a cooling process, and an inert gas is introduced into the recovery chamber 40. First gas introduction means 42a, second introduction means 42b for introducing an oxygen-containing gas, vacuum evacuation means 43 for discharging the gas in the recovery chamber 40, and the processing vessel 50 from the processing chamber into the recovery chamber 40 It has a carry-in port for carrying in, a discharge port 40a arranged at the lower part of the collection chamber 40, and a collection container 1 connected to the discharge port 40a. After introducing the inert gas, the processing container 50 is carried from the processing chamber into the recovery chamber 40 through the carry-in entrance, and after the pressure in the recovery chamber 40 is reduced by the vacuum exhaust means 43, the hydrogen crushed powder in the processing container 50 is recovered. Discharged into the chamber 40, hydrogen powder After the powder is discharged into the recovery chamber 40, an inert gas and / or an oxygen-containing gas is introduced into the recovery chamber 40 by the first gas introduction means 42a and / or the second gas introduction means 42b. After the inside is set to a predetermined pressure with an inert gas and / or an oxygen-containing gas, the rare earth magnet raw material alloy is recovered in the recovery container 1 from the outlet. Accordingly, when the hydrogen pulverized powder in the processing container 50 is discharged into the recovery chamber 40, the recovery chamber 40 is depressurized, so that the hydrogen pulverized powder falls without flying in the recovery chamber 40. It does not adhere to the inner wall surface of the chamber 40. As described above, the hydrogen pulverized powder adhering to the inner wall surface of the recovery chamber 40 is oxidized when the inside of the recovery chamber 40 is opened to the outside air by carrying out the processing container 50 or the like, and mixed into the hydrogen pulverized powder in the next hydrogen pulverization process. Therefore, even in continuous operation, low-oxygen hydrogen pulverized powder can be stably mass-produced, and the magnetic properties of the rare earth magnet can be improved. In addition, when discharging from the discharge port 40a to the collection container 1, smooth discharge can be performed because the inside of the collection chamber 40 is set to a predetermined pressure with an inert gas. Therefore, a large-scale device is not required.
Further, in the present embodiment, the recovery chamber 40 has reversing means 44 for turning the processing vessel 50 upside down. The processing vessel 50 has an opening on the upper surface, and the rare earth magnet raw material alloy in the processing vessel 50 Is discharged by upside down by a reversing means. Therefore, compared to the case where the lower part of the processing vessel 50 is opened and the hydrogen pulverized powder is dropped, the hydrogen pulverized powder is less likely to remain around the opening and the lid, and the pressure is further reduced. There is no influence of the pulverization of the hydrogen pulverized powder caused by the air flow.

Further, in this embodiment, the processing container 50 has a lid 51 that covers the opening of the processing container 50. When the vacuum exhaust means 43 depressurizes, the cover 51 covers the opening, and the vacuum exhaust means 43 places the inside of the collection chamber 40. After the pressure is reduced, the lid 51 is removed from the opening before the upside down by the inversion means 44. Accordingly, it is possible to prevent the hydrogen pulverized powder from being discharged together with the gas during the decompression operation, and the hydrogen pulverized powder does not rise due to the generation of an air flow when the lid 51 is released.
In the present embodiment, the hydrogen storage step by the hydrogen storage chamber 10, the heating step by the heating chamber 20, and the cooling step by the cooling chamber 30 can be performed with the opening of the processing container 50 covered with the lid 51. Furthermore, the hydrogen pulverized powder is not discharged together with the gas during the decompression in the recovery chamber 40.
In the present embodiment, the rare earth magnet raw material alloy is discharged from the processing vessel 50 under reduced pressure of 1000 Pa to 1 Pa in the recovery chamber 40, thereby eliminating the generation of airflow in the recovery chamber 40. In addition, it is possible to prevent the hydrogen pulverized powder from adhering to the inner wall surface of the recovery chamber 40 and the like.
Further, in this embodiment, the air in the recovery container 1 is replaced with an inert gas in advance so that the oxygen concentration is 20 ppm or less, and the predetermined pressure in the recovery chamber 40 is the same as the pressure in the recovery container 1. By doing so, oxidation in the collection container 1 can be prevented, and the hydrogen pulverized powder can be easily discharged from the collection chamber 40 to the collection container 1.

Next, a more detailed configuration and operation of the collection chamber described with reference to FIG. 6 will be described.
FIG. 7 is a front view of the main part of a recovery chamber (recovery device of hydrogen pulverized powder of a rare earth magnet raw material alloy) in the hydrogen pulverizer, FIG. 8 is a side view of the main part of the recovery chamber, and FIG. FIG. 10 is a top view of the main part of the recovery chamber.
8 to 10, the blocking door 41, the first gas introduction unit 42a, the second gas introduction unit 42b, and the vacuum exhaust unit 43 are not illustrated.
The lower portion of the recovery chamber 40 has a funnel shape, and the accumulated hydrogen pulverized powder of the rare earth magnet raw material alloy is recovered from the discharge port 40a of the lower funnel shape to the recovery container 1 (not shown in FIGS. 7 to 10). Can be discharged. A valve 60 is provided at the discharge port 40a. The recovery container 1 is also provided with a valve (not shown). An air hammer may be provided in the lower part of the collection chamber 40.
The collection chamber 40 has a conveyor means 45 that carries the processing container 50 in and out. The conveyor means 45 is composed of a plurality of rollers. Further, the recovery chamber 40 has a reversing means 44 described later and a pressure measuring means for measuring the pressure in the recovery chamber 40.
In the collection chamber 40, movement preventing means 46a and 46b for preventing the movement of the processing container 50 in the conveying direction of the conveyor means 45 are provided on both sides in the conveying direction of the processing container 50. These movement preventing means 46a and 46b are arranged between the rollers constituting the conveyor means 45, and are provided so as to be able to appear on the processing container 50 side from the conveying surface by the rollers. The movement preventing means 46 a is provided on the front side in the transport direction of the processing container 50, and the blocking means 46 b is provided on the rear side in the transport direction of the processing container 50.

FIG. 9 shows the movement blocking means 46a. The movement preventing means 46a has a sliding shaft 46c and a cam plate 46d. One end of the cam plate 46d is pivotally supported by the sliding shaft 46c, and the other end serves as a blocking portion. Accordingly, the cam plate 46d is rotated about the rotation shaft 46e by the movement of the sliding shaft 46c, so that the blocking portion appears and disappears with respect to the conveying surface of the conveyor means 45. The movement blocking means 46b has the same configuration. There are no particular limitations on the shape, size, number, etc. of the movement blocking means 46a, 46b.
Further, in the collection chamber 40, separation prevention means 47 that prevents the processing container 50 from being detached from the conveyor means 45 is provided on both sides in a direction orthogonal to the loading direction of the processing container 50. The separation preventing means 47 is provided on the opening side of the processing container 50. A flange 52 is provided on the outer periphery in the vicinity of the opening of the processing container 50.
The separation preventing means 47 is disposed so as to be positioned on the upper portion of the flange portion 52 in a state where the processing container 50 is loaded. Here, for example, the separation preventing means 47 is configured to have an L-shaped cross-sectional shape. In the present embodiment, the flange 52 provided in the processing container 50 is disposed on the outer periphery in the vicinity of the opening of the processing container 50, but the processing container 50 has the longitudinal direction of the pair of flanges 52 as the transport direction. It is good also as a structure arrange | positioned on both sides of.

The reversing unit 44 includes a base 44a that holds the conveyor unit 45 and the movement preventing units 46a and 46b, a rotating shaft 44b that rotates the base 44a, and a motor 44c that drives the rotating shaft 44b.
The base 44a is constituted by a pair of opposed wall portions perpendicular to the roller shaft of the conveyor means 45, and the rotating shaft 44b is pivotally supported by the pair of opposed wall portions. Further, the separation preventing means 47 is also provided on the opposing surface of the opposing wall surface. The rotating shaft 44b for rotating the base 44a and the main rotating shaft for rotating a plurality of rollers constituting the conveyor means 45 are coaxially arranged.
Above the collection chamber 40, there is a lid opening / closing means 48 having an engagement piece 48a. The engagement piece 48 a is engaged with an engagement piece 53 provided on the upper surface of the lid 51. By the transfer operation in which the processing container 50 is carried into the recovery chamber 40 from the cooling chamber 30, the upper engagement piece 48 a in the recovery chamber 40 is engaged with the engagement piece 53 on the upper surface of the lid 51, and the engagement piece 48 a is moved upward. The lid 51 can be removed from the opening by moving to.
Here, for example, the engagement piece 48a and the engagement piece 53 are configured such that one engagement piece has a T-shaped cross-sectional shape and the other engagement piece has a substantially C-shaped cross-sectional shape. . In this embodiment, the engagement piece 53 has a substantially C-shaped cross section, the engagement piece 48a has an inverted T-shaped cross section, and the engagement piece 48a and the engagement piece 53 Is formed of a rail-like member extending in one direction. In the present embodiment, the slit is formed by a pair of members having an inverted L-shaped cross section, which is referred to as a substantially C shape.

In the present embodiment, a lid opening / closing means 48 is provided above the collection chamber 40, and the engagement piece 48 a and the engagement piece 53 are moved by a transfer operation in which the processing container 50 is carried into the collection chamber 40 from the cooling chamber 30. The lid 51 is removed from the opening by engaging and moving the engagement piece 48a upward. Thus, in order to engage the engagement piece 48a and the engagement piece 53 using the transfer operation carried into the collection chamber 40, the lid opening / closing means 48 simply moves the engagement piece 48a upward. The lid 51 can be removed from the opening.
In this embodiment, the reversing unit 44 reverses the processing container 50 together with the conveyor unit 45 in a state where the processing container 50 is placed on the conveyor unit 45. Thus, by inverting the conveyor means 45 together with the processing container 50, the hydrogen crushed powder discharged from the processing container 50 does not adhere to the conveyor means 45, and the hydrogen crushed powder reliably falls to the lower part of the collection chamber 40. Can be made. Further, since the rotation shaft 44b for rotating the base 44a holding the conveyor means 45 and the main rotation shaft for rotating the plurality of rollers constituting the conveyor means 45 are coaxially arranged, the reversal is easily performed. be able to.

In the reversing operation, first, the processing container 50 is rotated 180 degrees, and the opening of the processing container 50 is directed directly below. Thereafter, it is desirable to apply one or more swings. For example, after rotating 180 degrees and directing the opening of the processing container 50 directly below, it is further rotated 45 degrees, and the position rotated 45 degrees is reversed by 90 degrees. By swinging in this way, a small amount of hydrogen pulverized powder deposited on the pipe penetrating the processing vessel 50 can be completely dropped.
The reversing operation is controlled so that the operation is started based on the pressure information measured by the pressure measuring means for measuring the pressure in the recovery chamber 40 after the vacuum exhaust means 43 of the recovery chamber 40 is operated. . For example, the reversing operation is started at a pressure of 1000 Pa or less. Various pressure gauges and vacuum gauges can be used as the pressure measuring means. As a result, the hydrogen pulverized powder falls without fluttering in the recovery chamber 40 during reversal, so that adhesion to the inner wall surface of the recovery chamber 40 and the like can be prevented.
As shown in FIG. 7, the recovery chamber 40 is provided with an oxygen concentration measuring means 49b for measuring the oxygen concentration together with a pressure measuring means 49a for measuring the pressure in the recovery chamber 40. Controlling the pressure in the recovery chamber 40 based on the pressure information measured by the pressure measuring means 49a, and controlling the oxygen concentration in the recovery chamber 40 based on the oxygen concentration information measured by the oxygen concentration measuring means 49b. Thus, the oxygen content of the recovered hydrogen pulverized powder can be controlled. Further, the reversing operation may be controlled based on the pressure information in the recovery chamber 40, or in some cases, the reversing operation may be controlled using only the oxygen concentration measuring means.

As shown in FIG. 7, on the side where the collection container 1 of the valve 60 is disposed, first gas introduction means 42a for introducing an inert gas into the collection container 1 and second gas introduction for introducing an oxygen-containing gas. Means 42b and oxygen concentration measuring means 49b for measuring the oxygen concentration in the collection container 1 are provided. As described above, in order to further increase the oxygen concentration of the hydrogen pulverized powder adjusted in the recovery chamber 40, an inert gas and / or an oxygen-containing gas is introduced into the recovery container 1, and the atmosphere in the recovery container 1 Can be adjusted to have a predetermined oxygen concentration to control the oxygen content of the hydrogen pulverized powder.
In this embodiment, the movement preventing means 46a and 46b are provided on the front side and the rear side of the processing container 50 in the transport direction, respectively, and the removal preventing means 47 for preventing the processing container 50 from being detached from the conveyor means 45 is provided. When the reversing means 44 is reversed, the processing container 50 can be held at a predetermined position with respect to the conveyor means 45 by the pair of movement preventing means 46a and 46b and the separation preventing means 47. The reversal operation can be reliably performed even in the space.
In the present embodiment, the movement preventing means 46a and 46b are provided so as to be able to protrude and retract from the rollers constituting the conveyor means 45 toward the processing container 50, so that the apparatus can be downsized in order to use the gap between the rollers. Since it is easy to maintain the positional relationship with the roller accurately, the processing container 50 can be reliably held.
In the present embodiment, the separation preventing means 47 is disposed so as to be positioned on the upper portion of the flange portion 52 in a state in which the processing container 50 is loaded. In this way, by forming the flange portion 52, the flange portion 52 and the detachment preventing means 47 can be made to correspond to each other by the conveying operation, and the processing container 50 can be held at a predetermined position.
In the present embodiment, a dry air generator (not shown) is disposed in the front stage of the second gas introduction means 42b, and the oxygen-containing gas supplied from the second gas introduction means 42b is the outlet air. The dew point under pressure is 10 ° C. (atmospheric pressure dew point−17 ° C.). As a result, when air is used as the oxygen-containing gas, the influence of moisture contained in the air on the oxidation of the hydrogen pulverized powder can be suppressed, and the oxygen content of the hydrogen pulverized powder can be reduced to a predetermined value. It becomes possible to adjust accurately.

Next, the configuration and operation of the valve described in FIG. 6 will be described.
FIG. 9 is a block diagram showing the operation of a valve provided at the outlet of the recovery chamber.
FIG. 4A shows a state in which the valve is open, FIG. 5B shows a state in the middle of the valve closing operation, and FIG. 4C shows a state in which the valve is closed.
The valve 60 includes an annular expansion member 62 disposed on the inner peripheral surface of the cylindrical member 61, and a disk member 63 that uses the radial direction of the cylindrical member 61 as a rotation shaft 63a.
The annular expansion member 62 may be a member that can be elastically deformed by its own material or structure, but is preferably expandable by an external gas pressure.
The disk member 63 is rotated by the rotation shaft 63a, and is opened in the state shown in FIG. Further, the disk member 63 and the annular expansion member 62 are hermetically sealed by causing the annular expansion member 62 to be inflated and deformed after the cylindrical member 61 is moved to the closing position in the state shown in FIG. .
According to the valve 60 of the present embodiment, it is possible to eliminate the influence of adhesion of the hydrogen pulverized powder and maintain hermeticity.
When the oxygen concentration in the recovery container 1 is 20 ppm or less and the pressure in the recovery chamber 40 becomes equal to the pressure in the recovery container 1 by the first gas introduction means 42a of the recovery chamber 40, the valve 60 Control is performed so that the opening / closing operation can be performed. Therefore, the oxidation in the collection container 1 can be prevented, and the hydrogen pulverized powder can be easily discharged from the collection chamber 40 to the collection container 1. When the oxygen concentration in the recovery container 1 is adjusted to an oxygen concentration exceeding 20 ppm, the opening / closing operation of the valve 60 is controlled according to the pressure and the oxygen concentration at that time.

In the above embodiment, the case where the RTB-based magnet raw material alloy is used as the rare earth-based magnet raw material alloy has been described. However, the oxygen reduction step of the hydrogen pulverized powder of the Sm-Co-based magnet raw material alloy is described. It can also be applied to.
As a raw material alloy for rare earth magnets used in the hydrogen pulverizing apparatus according to the present embodiment, Nd23.24, Pr6.44, Dy0.55, B0.92, Al0.09, Ga0.08, A quenched alloy was prepared by a strip casting method using a composition adjusted to be Co2.00 and Cu0.10 (each mass%).
Then, 400 kg of this strip cast alloy was put into this apparatus, and the hydrogen pulverized powder of the rare earth magnet raw material alloy was recovered in the recovery container 1.
On the other hand, a comparative experiment was performed using the same material and the same apparatus. The hydrogen pulverized powder was dropped into the collection chamber without reducing the pressure when the inverting means was turned upside down.
In addition, the internal pressure at the time of inversion in Example 1 was set to 5 Pa, and the pressure at the time of argon gas introduction after inversion was set to the same pressure as the atmospheric pressure. In Comparative Example 1, no vacuum evacuation was performed at the time of reversal, and the pressure was made the same as the atmospheric pressure by introducing argon gas from the time of reversal.
In Example 1, the hydrogen pulverized powder remaining in the recovery chamber 40 was collected, and the hydrogen pulverized powder was 0.1 g or less. In the comparative experiment, 100 g of hydrogen pulverized powder was recovered from the recovery chamber 40.

Example 2
Using a hydrogen crusher according to the present invention, a strip cast alloy having an oxygen content of 200 ppm is used as a raw material alloy, a hydrogen occlusion process, a heating process, and a cooling process are performed, and the processing chamber is turned upside down in the recovery chamber at a pressure of 5 Pa. The hydrogen pulverized powder was discharged.
Next, in order to bring the inside of the collection chamber to the same pressure (atmospheric pressure) as the collection container, argon gas was introduced, and then the hydrogen pulverized powder was collected in the collection container.
As a result of measuring the oxygen content of the recovered hydrogen pulverized powder by an inert gas melting infrared absorption method, the oxygen content was 500 ppm.

Example 3
The hydrogen pulverized powder was recovered in the same manner as in Example 2 except that air having an atmospheric dew point of −17 ° C. was introduced instead of introducing argon gas.
As a result of measuring the oxygen content of the recovered hydrogen pulverized powder by the same method as in Example 2, the oxygen content was 1500 ppm.

  The present invention can be used in a method and apparatus for manufacturing a rare earth magnet.

DESCRIPTION OF SYMBOLS 1 Recovery container 1b Water cooling jacket 1d Bucket 2 Shut-off door 10 Hydrogen storage room 11 Shut-off door 12 Inert gas introduction means 13 Vacuum exhaust means 14 Hydrogen introduction means 15 Conveyor means 20 Heating chamber 21 Shut-off door 22 Inert gas introduction means 23 Vacuum exhaust Means 24 Heating means 25 Conveyor means 30 Cooling chamber 31 Shut-off door 32 Inert gas introduction means 33 Vacuum exhaust means 34 Cooling means 35 Conveyor means 40 Collection chamber 41 Shut-off door 42a First gas introduction means 42b Second gas introduction means 43 Vacuum evacuation means 44 Reversing means 45 Conveyor means 46a, 46b Movement prevention means 47 Detachment prevention means 48a Engagement piece 49a Pressure measurement means 49b Oxygen concentration measurement means 50 Processing vessel 51 Lid 52 Hook 53 Engagement piece 60 Valve 61 Cylindrical shape Member 62 annular expansion member 63 disk portion

Claims (26)

A hydrogen storage step of storing hydrogen in a rare earth magnet raw material alloy contained in a processing vessel;
A heating step of heating and dehydrogenating the rare earth magnet raw material alloy pulverized by hydrogen storage;
A cooling step of cooling the heated rare earth magnet raw material alloy;
A recovery step of recovering the cooled hydrogen pulverized powder of the rare earth magnet raw material alloy in a recovery container;
A lubricant addition step of adding a lubricant to the hydrogen pulverized powder in the recovery container containing the recovered hydrogen pulverized powder;
A mixing step of mixing the hydrogen pulverized powder and the lubricant while cooling the recovery container containing the hydrogen pulverized powder to which the lubricant is added;
A method for producing a hydrogen pulverized powder of a raw material alloy for rare earth magnets, comprising:
The recovery step is performed in a recovery chamber connected to one or a plurality of processing chambers that perform the hydrogen storage step, the heating step, and the cooling step,
A first gas introduction means for introducing an inert gas;
A second gas introduction means for introducing an oxygen-containing gas;
A vacuum exhaust means for exhausting the gas in the recovery chamber;
A carry-in port for carrying the treatment container from the treatment chamber into the collection chamber;
A discharge port disposed in a lower portion of the recovery chamber;
The recovery container connected to the outlet,
After introducing an inert gas into the recovery chamber by the first gas introduction means,
Carrying the processing container from the processing chamber into the recovery chamber through the inlet;
After depressurizing the collection chamber by the vacuum exhaust means,
Discharging the hydrogen pulverized powder in the processing container into the recovery chamber;
After discharging the hydrogen pulverized powder into the recovery chamber,
An inert gas and / or an oxygen-containing gas is introduced into the recovery chamber by the first gas introduction means and / or the second gas introduction means, and the recovery chamber is set to a predetermined pressure and a predetermined oxygen concentration. A method for producing hydrogen pulverized powder of a raw material alloy for rare earth magnets, wherein the hydrogen pulverized powder is collected in the collection container.   The recovery chamber has a reversing unit that flips the processing container upside down. The processing container has an opening on the top surface, and discharges the hydrogen pulverized powder in the processing container up and down by the reversing unit. The method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to claim 1, wherein the method is performed by reversal.   3. The hydrogen pulverization of the rare earth-based magnet raw material alloy according to claim 2, wherein after the reversing means is turned upside down, the reversing means performs a swinging motion with the opening directed downward. Powder manufacturing method.   The processing container has a lid that covers the opening of the processing container, covers the opening with the lid when depressurizing by the vacuum evacuation means, and after the collection chamber is depressurized by the vacuum evacuation means, The method for producing a hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to claim 2 or 3, wherein the lid is removed from the opening before the reversing means is turned upside down.   The raw material alloy for a rare earth magnet according to claim 4, wherein the hydrogen storage step, the heating step, and the cooling step are performed in a state where the opening of the processing container is covered with the lid. A method for producing hydrogen pulverized powder.   The rare earth magnet raw material alloy according to any one of claims 1 to 5, wherein the hydrogen pulverized powder is discharged from the processing container under reduced pressure of 1000 Pa to 1 Pa in the recovery chamber. A method for producing hydrogen pulverized powder.   The said predetermined pressure in the said collection | recovery chamber is made the same pressure as the pressure in the said collection | recovery container by which oxygen concentration was previously 20 ppm or less by introduction | transduction of the inert gas. The manufacturing method of the hydrogen pulverized powder of the raw material alloy for rare earth magnets described in 1.   The predetermined pressure in the recovery chamber is set to be the same pressure as the pressure in the recovery container in which the oxygen concentration has become an oxygen concentration exceeding 20 ppm in advance by introducing an inert gas and / or an oxygen-containing gas. The manufacturing method of the hydrogen ground powder of the raw material alloy for rare earth magnets in any one of Claims 1-6.   The method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to claim 1, wherein the lubricant has a melting point of 100 ° C. or less.   The method for producing a hydrogen pulverized powder of a rare earth magnet raw material alloy according to claim 1 or 9, wherein the lubricant is added by a bucket disposed in the recovery container.   The rare earth magnet raw material alloy hydrogen pulverized powder according to any one of claims 1, 9, and 10, wherein the recovery container is cooled by a water cooling jacket disposed on an outer surface of the recovery container. Manufacturing method.   The method for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to claim 11, wherein a coolant of 20 ° C. to 30 ° C. is supplied to the water cooling jacket.   The rare earth magnet raw material alloy according to any one of claims 1 and 9, wherein the hydrogen pulverized powder and the lubricant are mixed by rotating the recovery container itself. A method for producing hydrogen pulverized powder. One or a plurality of processing chambers for storing a rare earth-based magnet raw material alloy contained in a processing vessel having an opening on the upper surface, a hydrogen storage process, a heating process, and a cooling process, and a recovery chamber connected to the processing chamber. In the recovery chamber, a first gas introduction means for introducing an inert gas, a second gas introduction means for introducing an oxygen-containing gas, a vacuum exhaust means for discharging the gas in the recovery chamber, The processing container has a carry-in port for carrying in the processing chamber from the processing chamber to the collection chamber, and a discharge port arranged at a lower portion of the collection chamber, and the inside of the processing vessel carried into the collection chamber from the processing chamber An apparatus for producing hydrogen pulverized powder of rare earth magnet raw material alloy that discharges hydrogen pulverized powder of the rare earth magnet raw material alloy into the recovery chamber and collects the rare earth magnet raw material alloy into the recovery container,
The recovery container is provided with a bucket for storing a lubricant in the recovery container and a water cooling jacket for cooling the recovery container on the outer surface of the recovery container,
The recovery chamber includes reversing means for turning the processing container upside down and pressure measuring means for measuring the pressure in the recovery chamber, and information on pressure measured by the pressure measuring means after operating the evacuation means. The rare earth magnet raw material is characterized in that the reversing means is operated to turn the processing vessel upside down to discharge the hydrogen pulverized powder of the rare earth magnet raw material alloy in the processing vessel into the recovery chamber. Production equipment for alloy hydrogen pulverized powder.   The apparatus for producing hydrogen pulverized powder of a raw material alloy for rare earth magnets according to claim 14, further comprising oxygen concentration measuring means for measuring the oxygen concentration in the recovery chamber.   16. The apparatus for producing hydrogen pulverized powder of a rare earth-based magnet raw material alloy according to claim 14 or 15, wherein the pressure measured by the pressure measuring means is 1000 Pa or less.   The said inversion means further rocks | fluctuates the said processing container in the state which turned the said processing container upside down and turned the said opening part of the said processing container downward. An apparatus for producing hydrogen pulverized powder of a raw material alloy for rare earth magnets as described.   The processing container has a lid that covers the opening of the processing container and a lid opening / closing means for removing the lid, and the lid opening / closing means is provided in an engagement piece provided in the lid and the collection chamber. 18. The lid according to claim 14, wherein the lid is detached by engaging the engagement piece formed and moving the engagement piece provided in the collection chamber upward. Production equipment for hydrogen pulverized powder of rare earth magnet raw material alloys.   The engaging piece provided in the lid is arranged at the upper part of the lid, and the engaging piece provided in the collecting chamber is arranged in the upper part of the collecting chamber. 19. The production of hydrogen pulverized powder of a rare earth magnet raw material alloy according to claim 18, characterized in that it has a T-shaped cross-sectional shape and the other engaging piece has a substantially C-shaped cross-sectional shape. apparatus.   20. The recovery chamber includes conveyor means for carrying the processing container from the processing chamber, and the reversing means reverses the processing container together with the conveyor means. An apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to claim 1.   Movement prevention means for preventing movement of the processing container at the time of reversal are provided on both sides of the conveyor means in the processing container transport direction, respectively, and on both sides of the conveyor means in a direction orthogonal to the processing container carry-in direction, Detachment prevention means for preventing detachment of the processing container from the conveyor means is provided, respectively, and when the reversing means is reversed, the processing container with respect to the conveyor means by the pair of movement prevention means and the pair of separation prevention means. 21. The apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to claim 20, wherein the is held at a predetermined position.   The rare earth magnet according to claim 21, wherein the conveyor means is composed of a plurality of rollers, and the movement preventing means is provided so as to be able to protrude and retract on the processing container side from between the rollers. Production equipment for hydrogen pulverized powder of raw material alloy.   The said detachment preventing means has an L-shaped cross-sectional shape, and is disposed so as to be positioned above an eaves portion provided on the outer periphery in the vicinity of the opening of the processing container. An apparatus for producing hydrogen pulverized powder of a raw material alloy for rare earth magnets according to 22.   The discharge port has a valve, and the valve is composed of an annular expansion member disposed on an inner peripheral surface of the cylindrical member, and a disk member having the radial direction of the cylindrical member as a rotation axis. 24. The apparatus for producing hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to any one of claims 14 to 23.   The apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to claim 14, wherein the lubricant is discharged into the collection container by inverting the bucket in the collection container.   The apparatus for producing a hydrogen pulverized powder of a raw material alloy for a rare earth magnet according to claim 14, wherein a coolant at 20 ° C to 30 ° C is supplied to the water cooling jacket on the outer surface of the recovery container.