JPH09251912A - Rare earth magnet powder producing apparatus and heat treating apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a rare earth magnet powder producing apparatus and a heat treating apparatus therefor whereby the temp. at hydrogen treatment of a rare earth magnet raw material is stabilized to produce a high quality rare earth type magnet with little magnetic characteristic dispersion. SOLUTION: A rare earth magnet raw material 2 is equally held in reaction tubes 10. A hold tube 27 holding a dummy material 25 having the same compsn. as the material 2 is put near the tubes 10 and heated at about 800 deg.C by a heater 4 to occlude hydrogen by the material 2 to generate the heat while hydrogen is discharged from the dummy material 25 to absorb the heat, and then hydrogen occluded by the material 2 is discharged to absorb the heat while hydrogen is occluded by the material 25 to generate the heat. The exothermic and endothermic actions are apt to cancel out, thus suppressing a great temp. variation of the material 2.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the production of rare earth magnet powder for improving the magnetic properties of the rare earth magnet raw material by causing the rare earth magnet raw material to absorb hydrogen and then releasing hydrogen from the rare earth magnet raw material. The present invention relates to an apparatus for producing a rare earth magnet powder that can be used in and a heat treatment apparatus that can be used for the apparatus.

[0002]

2. Description of the Related Art In recent years, rare earth magnet powders having excellent magnetic properties have been actively used. As a technique for producing a rare-earth magnet powder having excellent magnetic properties, a hydrogen-absorbing step of heating the rare-earth-based magnet raw material to a high-temperature region, for example, 750 to 950 ° C., and storing hydrogen in the rare-earth-based magnet raw material, There is known a technique of sequentially performing a hydrogen releasing step of forcibly releasing hydrogen from a magnet raw material.

[0003] In this technique, it is known that the hydrogen treatment temperature in the hydrogen storage step and the hydrogen release step varies, and it is difficult to obtain rare-earth magnet powder having excellent magnetic properties. By the way, according to this rare earth magnet raw material, during the hydrogen treatment, heat is generated as hydrogen is absorbed, and heat is absorbed as hydrogen is released. Therefore, it is not always easy to make the temperature of the rare earth magnet raw material uniform with high accuracy in the hydrogen storage step or the hydrogen release step.

Therefore, conventionally, by using a heat storage material capable of storing heat and bringing the heat storage material into contact with the rare earth magnet raw material, heat is stored in the heat storage material when the rare earth magnet raw material generates heat, and is stored when the rare earth magnet raw material absorbs heat. Has been developed to dissipate heat and thereby make the temperature of the rare earth magnet raw material uniform. However, even the heat storage material is not yet enough to reduce the variation in the temperature of the rare earth magnet raw material.

Japanese Patent Application Laid-Open No. 5-163510 discloses that
A technique using radiant heat, which makes it easy to make the heating temperature uniform when a rare earth magnet raw material is heated to a high temperature range, is disclosed. However, this is not enough to make the temperature of the rare earth magnet raw material uniform, and causes variations in magnetic characteristics due to variations in the hydrogen treatment temperature. Japanese Patent Laid-Open No. 5-
JP-A-171203 and JP-A-5-171204 disclose a technique in which a hydrogen storage alloy is used as a hydrogen gas supply source when a rare earth magnet is subjected to hydrogen treatment in a high temperature range. In this case, since the hydrogen gas to be subjected to the hydrogen treatment can be highly purified, it is possible to prevent the magnetic material from being contaminated by impurities contained in the hydrogen gas, and it is possible to avoid variations in magnetic characteristics due to impurity contamination. However, even the technique disclosed in this publication is not sufficient for making the temperature of the rare earth magnet raw material uniform during the hydrogen treatment, and causes a decrease in magnetic properties due to the variation in the hydrogen treatment temperature.

[0006]

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned circumstances, and has an endothermic action that is substantially in synchronism with the heat generation of the rare earth magnet raw material and an exothermic action that is approximately in synchronism with the heat absorption of the rare earth magnet raw material. At least one of them is made of a thermal functional material so that the temperature of the rare earth magnet raw material is made uniform and stable in the hydrogen treatment in which the rare earth magnet raw material is retained in a high temperature range and then hydrogen is absorbed and then released. The present invention is advantageous in avoiding variations in magnetic properties of rare earth magnet powders, and thus provides a rare earth magnet powder manufacturing apparatus and heat treatment apparatus suitable for mass production and industrialization of rare earth magnet powders. It is in.

[0007]

According to the present invention, there is provided a method for producing a rare earth magnet powder, comprising: a rare earth magnet raw material having a property of improving magnetic properties by absorbing hydrogen with heat generation and releasing hydrogen with heat absorption; A hydrogen storage step of being provided close to the rare-earth magnet raw material and using a heat functional material having at least one of endothermic property and heat-generating property, and storing hydrogen in the rare-earth magnetic raw material while heating the rare-earth magnetic raw material, A hydrogen releasing step of releasing hydrogen from the rare-earth magnet raw material while heating the rare-earth magnetic raw material, wherein the heat absorption and the hydrogen release substantially synchronized with the heat generation of the rare-earth magnetic raw material in the hydrogen storage step. At least one of the heat generation substantially synchronized with the heat absorption of the rare-earth-based magnet raw material in the process is performed by the thermal functional material.

[0008] The apparatus for producing a rare earth magnet powder of the present invention comprises:
A raw material holding portion for holding a rare earth magnet raw material having characteristics that magnetic characteristics are improved by absorbing hydrogen with heat generation and releasing hydrogen with heat absorption, which can be used for carrying out the above-described manufacturing method; A heating device for heating the rare-earth magnet raw material of the portion, a hydrogen gas feeding device for feeding hydrogen to the raw material holding portion and absorbing hydrogen in the rare-earth magnetic material of the raw material holding portion, and depressurizing the raw material holding portion. An exhaust device for releasing hydrogen from the rare-earth magnet raw material in the raw material holding unit, and a thermal functional material provided in close proximity to the rare-earth magnetic raw material in the raw material holding unit and holding a heat-absorbing and exothermic thermal functional material The holding unit and the heat absorbing material absorb heat of the rare earth-based magnet raw material in the raw material holding unit substantially in synchronization with the heat generation of the rare earth magnet raw material in the raw material holding unit. Means The one in which the features.

Further, the heat treatment apparatus of the present invention comprises a heating vessel forming a heating chamber, a sealed vessel arranged in the heating chamber for heating or cooling the heating chamber, and a hydrogen storage alloy arranged in the sealed vessel. And a hydrogen gas pressure control device for controlling the hydrogen gas pressure in the closed vessel. The rare-earth-based magnet raw material according to the present invention has characteristics in which magnetic properties (coercive force, residual magnetic flux density, etc.) are improved by absorbing hydrogen with heat generation and releasing hydrogen with heat absorption. Generally, RT-boron system, RT-M
The system can be adopted. R means a rare earth element, Y, L
a, Ce, Pr, Nd, Sm, Gd, Tb, Dy, H
o, Er, Tm, and Lu can be adopted. One or two of Nd and Pr may contain 50 at% of R. T means an iron group element, and at least one of Fe, Co, and Ni can be adopted.
% Can be included. M is an element for generating a tetragonal ThMn ₁₂ type compound, and Ti, V, Cr, and Mo can be employed.

[0010] As the rare earth magnet raw material according to the present invention, specifically, Nd-Co-Ga-B-Fe system, Nd-Fe-T
i-type, Nd-Fe-Ti-C-type, Nd-Fe-VC-type and the like can be adopted. In the present invention, the raw material holder may be composed of an appropriate number of pipes that divide the rare earth magnet raw material and hold it separately from each other. As the pipe body, generally, a large number of test pipe pipes and a large number of containers can be adopted. The number of tubes can be selected as appropriate, but can be, for example, three, four, five or more. Several tens or several hundreds may be used. The raw material holding portion such as a tube is preferably formed of a material having good heat conductivity and a small heat capacity, preferably a metal such as stainless steel. This is because it is advantageous for soaking the rare-earth magnet raw material.

The thermal functional material according to the present invention has at least one of endothermic property and exothermic property, and preferably has both endothermic property and exothermic property. As a typical thermal functional material, a hydrogen storage alloy can be exemplified. The hydrogen storage alloy raises the hydrogen gas partial pressure and generates heat when storing hydrogen. Conversely, by reducing the hydrogen gas partial pressure, the stored hydrogen is released and heat is absorbed. By using a hydrogen storage alloy as the heat functional material and adjusting the hydrogen gas partial pressure, both functions of heat generation and heat absorption can be exhibited. More specifically, a dummy material mainly composed of a rare earth magnet having the same composition or the same composition as the rare earth magnet raw material to be the rare earth magnet powder can be used as the thermal functional material.

Further, a transition metal which reacts with oxygen by increasing the partial pressure of oxygen gas to be oxidized when the partial pressure of oxygen gas is increased and decomposes to release oxygen when the partial pressure of oxygen gas is reduced can be used as the heat functional material. Furthermore, many metals that are oxidized and generate heat by reacting with oxygen can be used as the thermal functional material. The synchronizing means according to the present invention absorbs the heat-functional material substantially in synchronization with the heat generation of the rare-earth-based magnet raw material in the raw material holding unit, and heat-generates the heat-functional material in substantially synchronization with the heat absorption of the rare-earth-based magnet raw material in the raw material holding unit. To generate heat. Specifically, the adjustment of the partial pressure of the working gas that causes the working gas of the thermal functional material to be absorbed or released is substantially synchronized with the heat absorption or heat generation of the rare earth magnet raw material.

The heating container of the heat treatment apparatus of the present invention is a container for storing a material to be heat-treated. Specifically, as the heating container, a raw material holding unit of the above-described rare earth magnet powder manufacturing apparatus can be used. Further, this heating container can be used as a reaction container of a chemical reaction device or a heat treatment container of a heat treatment device. And it can be used for heating and / or cooling of the chemical raw material in the reaction vessel or the material to be heat treated in the heat treatment vessel.

[0014] The temperature control means of the heat treatment apparatus of the present invention comprises:
A temperature control means comprising: a closed container disposed in the heating chamber for heating or cooling the heating chamber; a hydrogen storage alloy disposed in the closed container; and a hydrogen gas pressure control device for controlling a hydrogen gas pressure in the closed container. Consists of As this closed container,
An example of the above-described thermal functional material holding unit of the apparatus for manufacturing a rare earth magnet powder is described. More specifically, a pipe containing a hydrogen storage alloy therein can be used as a sealed container. The hydrogen gas pressure control device controls the hydrogen gas pressure in the closed vessel by increasing or decreasing it. Specifically, it can be constituted by a hydrogen gas cylinder, a gas pressure control valve and / or a compressor joined to a closed container.

As the heating means of the heat treatment apparatus of the present invention, it is possible to employ a heating furnace having a storage chamber therein and having a heating portion inside or on the inner peripheral surface of a furnace wall forming the storage chamber. A plurality of heating vessels can be accommodated in the accommodation room of the heating furnace.

[0016]

According to the method of the present invention, when the rare earth magnet raw material stores hydrogen in the hydrogen storage step,
When the rare earth magnet raw material generates heat and hydrogen is released from the rare earth magnet raw material in the hydrogen releasing step, the rare earth magnet raw material absorbs heat. This improves the magnetic properties of the rare earth magnet raw material.

As described above, in the hydrogen storage step and the hydrogen release step, the rare-earth magnet raw material generates heat or absorbs heat, so that the temperature of the rare-earth magnet raw material may not be easily uniformed. In this respect, in the method of the present invention, in a state where the thermal functional material or the dummy material is brought close to the rare earth magnet raw material, the thermal functional material or the dummy material is absorbed substantially in synchronization with the heat generation of the rare earth magnetic raw material in the hydrogen storage step. Alternatively, the heat-generating material or the dummy material is caused to generate heat substantially in synchronization with the heat absorption of the rare-earth magnet raw material in the hydrogen releasing step.

Therefore, the temperature rise due to the heat generation of the rare earth magnet raw material in the hydrogen storage step is reduced by the heat absorption by the thermal functional material and the dummy material. Alternatively, the temperature decrease due to the endothermic heat of the rare earth magnet raw material in the hydrogen releasing step is reduced by the heat generated by the thermal functional material or the dummy material. Therefore, according to the method of the present invention, fluctuations in the temperature of the rare earth magnet raw material in the hydrogen storage step and the hydrogen release step can be suppressed. Therefore, it is advantageous for soaking the rare-earth magnet raw material, and it is advantageous for reducing or avoiding variation in the magnetic properties of the manufactured rare-earth magnet powder. Therefore, it can contribute to stabilization of the quality of the rare earth magnet powder, and is suitable for mass production and industrialization of the rare earth magnet powder.

By making the amount of the rare earth magnet raw material and the amount of the dummy material correspond to each other, the degree of heat generation by the rare earth magnet raw material and the degree of heat absorption by the thermal functional material or the dummy material can be made close to or equal to each other. It is advantageous to do so. Therefore, the fluctuation of the temperature of the rare-earth magnet raw material can be further suppressed in the hydrogen storage step and the hydrogen release step. As a result, it is advantageous for soaking the rare-earth magnet raw material, and it is advantageous for reducing or avoiding variation in the magnetic properties of the manufactured rare-earth magnet powder. Therefore, it is possible to contribute to stabilization of the quality of the rare earth magnet powder, and it is more suitable for mass production and industrialization of the rare earth magnet powder.

The synchronizing means absorbs the heat-functional material substantially in synchronization with the heat generation of the rare-earth magnet raw material in the raw material holding portion, and absorbs the heat-functional material substantially in synchronization with the heat absorption of the rare-earth magnetic material in the raw material holding portion. Can generate heat. Therefore, the method of the present invention described above can be performed. In other words, the fluctuation of the temperature of the rare earth magnet raw material is further suppressed in the hydrogen storage step and the hydrogen release step, which is advantageous for soaking the rare earth magnet raw material and reducing the variation in the magnetic characteristics of the manufactured rare earth magnet powder. It is advantageous to avoid or avoid.

Further, by dividing the rare-earth-based magnet raw material and holding it in an appropriate number of tubes, the rare-earth-based magnetic raw material can be separated and divided into small portions. Therefore, heat generation and heat absorption hardly affect each other between the adjacent small amounts of rare earth magnet raw material portions. Therefore, fluctuations in the temperature of the rare earth magnet raw material are further suppressed in the hydrogen storage step and the hydrogen desorption step, which is advantageous for soaking the rare earth magnet raw material, and reduces variations in the magnetic characteristics of the produced rare earth magnet powder. It is advantageous to avoid or avoid.

Further, the same number of heat function material holding portions as the number of tubes can be provided. And each thermal functional material holding | maintenance part is provided inside each tubular body. Thus, for each tube, the heat-absorbing material is absorbed substantially in synchronism with the heat generation of the rare-earth magnet raw material in the hydrogen storage step, or the heat-absorbing material is substantially synchronized with the heat absorption of the rare-earth magnetic material in the hydrogen releasing step Or to generate heat.

Since the fluctuation of the temperature of the rare-earth magnet raw material can be suppressed for each of the pipes divided into an appropriate number in this manner, it is more advantageous to equalize the temperature of the rare-earth magnet raw material, and the produced rare-earth magnet powder is produced. This is advantageous in reducing or avoiding variations in the magnetic characteristics of the magnetic head. Therefore, it is possible to contribute to stabilization of the quality of the rare earth magnet powder, and it is more suitable for mass production and industrialization of the rare earth magnet powder.

The heat treatment apparatus of the present invention can be used as a chemical reaction apparatus or a heat treatment apparatus which requires precise temperature control while producing a rare earth magnet powder. Direct heating and / or cooling is possible, making temperature control easier.

[0025]

Embodiments of the present invention will be described below with reference to the drawings. (Manufacturing Apparatus) FIG. 1 shows a principle diagram of a manufacturing apparatus according to this example. As shown in FIG. 1, the raw material holding unit 1 is composed of a suitable number of reaction tubes 10 which divide the rare earth magnet raw material 2 and hold them separately from each other. The material of the reaction tube 10 is stainless steel.

In this embodiment, the dummy material 2 is used as the thermal functional material.
5 is used. As the dummy material 25, a material having the same kind, that is, the same composition as the rare earth magnet raw material 2 is used. Dummy material 25
Are held inside a dummy material holding tube 27 as a heat functional material holding portion. The dummy material holding tube 27 is the reaction tube 1
The same number as 0 is provided, and is provided inside the reaction tube 10. Therefore, the dummy material 25 in the dummy material holding tube 27 and the rare earth magnet raw material 2 in the reaction tube 10 are arranged close to each other. The material of the dummy material holding tube 27 is stainless steel.

The first branching device 3 constitutes a hydrogen supply passage to each reaction tube 10 and a hydrogen release passage from each reaction tube 10. Therefore, the first branching device 3 is composed of a number of first branch passages 30 charged in each reaction tube 10 and a first concentrated passage 31 connecting the first branch passages 30. In this example, the material, diameter, length, volume, and the like of each reaction tube 10 are basically made uniform to ensure the synchronization of the hydrogen treatment in each reaction tube 10. The flow path diameter and the flow path length of the path 30 are basically equal.

The second branching device 7 includes the dummy material holding tubes 2
7 and a hydrogen release passage from each dummy material holding pipe 27. Therefore, the second branching device 7 is composed of a large number of second branch paths 70 charged in each dummy material holding pipe 27 and a second concentrated path 71 connecting the second branch paths 70. . In this example, the material, diameter, length, volume, and the like of the dummy material holding tubes 27 are basically equalized in order to ensure the synchronization of the hydrogen treatment in each dummy material holding tube 27. Second branch 70
Are basically equal to each other.

The heating device 4 heats the rare earth magnet raw material 2 and the dummy material 25, and has a heating chamber 40 equipped with a heating element. The temperature of the heating chamber 40 is controlled by a temperature control device 45. The hydrogen gas supply device 5 has a function of supplying hydrogen to the rare-earth magnet raw material 2 and the dummy material 25 to occlude them. The hydrogen gas supply device 5 includes a hydrogen cylinder 50 as a hydrogen source, a purifier 51 for removing impurities of hydrogen gas, a first switching valve 52 as a three-way valve, and a first accumulator 53 from the hydrogen cylinder 50. Via a first supply passage 54 leading to the first switching valve 52 via a second switching valve 56 which is a three-way valve; and a second supply passage 58 leading from the hydrogen cylinder 50 via the second accumulator 57 to the second switching valve 56.
And The first switching valve 52 is connected to the first concentrated path 31 of the first branch device 3. The second switching valve 56 is connected to the second concentrated path 71 of the second branch device 7.

The exhaust device 6 functions to release hydrogen from the rare-earth magnet raw material 2 in the reaction tube 10 by reducing the pressure in the reaction tube 10, and to reduce the pressure in the dummy material holding tube 27 to reduce the dummy material 2.
5 has a function of releasing hydrogen. Therefore, the exhaust device 6 includes the first vacuum pump 60, the first exhaust passage 61 connected to the first switching valve 52, the second vacuum pump 65, and the second vacuum pump 65.
And a second exhaust path 66 connected to the switching valve 56.

As can be understood from FIG. 1, the operation of the temperature control device 45, the switching of the switching valves 52 and 56, and the operation of the vacuum pumps 60 and 65 are controlled by the control device 98 via signal lines. As can be understood from the description below,
The control device 98 synchronizes the heat generation effect of the rare earth magnet raw material 2 with the occlusion of hydrogen and the heat absorption operation of the dummy material 25 with the release of hydrogen. Further, the control device 98 controls the endothermic effect of the rare earth magnet raw material 2 accompanying the release of hydrogen and the dummy material 25.
Is performed in synchronization with the heat generation effect accompanying the hydrogen occlusion. Therefore, the control device 98 functions as a synchronization unit.

(Hydrogen Storage Step) In this embodiment, the temperature is 250 ° C.
The rare earth magnet raw material 2 is preliminarily treated to occlude hydrogen and then release hydrogen to change from a massive form to a granular form (for example, about 2 to 4 mm). Then, the rare earth magnet raw material 2 is uniformly held in each reaction tube 10. The holding amount of the magnet raw material 2 per one reaction tube 10 can be appropriately selected, but can be, for example, about 0.5 to 5 kg. The magnet raw material 2 is a Nd-Co-Ga-B-Fe-based material, and its composition is specifically at% in Nd of 12.3%,
Co is 11.5%, B is 6.0%, Ga is 1.7%, inevitable impurities, and the balance is substantially Fe.

In this embodiment, a dummy material 25 in which hydrogen has been stored in advance is used. Then, the dummy material 25 is held in each dummy material holding tube 27. Rare earth magnet raw material 2
Each of the reaction tubes 10 in the state of holding the
At the same time, it is charged into the heating chamber 40 of the heating device 4. Thus, the heating device 4 heats the rare-earth magnet raw material 2 in the reaction tube 10 and the dummy material 25 in the dummy material holding tube 27 to a predetermined temperature range.

The temperature of the rare-earth magnet raw material 2 is controlled by the thermocouple 4
i, and the temperature of the dummy material 25 is measured by a thermocouple 4k (see FIG. 2). In this step, the control device 98
By operating the first switching valve 52, the first exhaust path 61
And the first concentrated path 31 are not communicated, and the first feed path 54 and the first concentrated path 31 are communicated. As a result, the high-pressure hydrogen gas press-fitted into the hydrogen gas supply device 5
The water is supplied to each reaction tube 10 via the supply path 54, the first switching valve 52, the first concentration path 31, and the first branch path 30.

As described above, in the hydrogen storage step, the rare-earth magnet raw material 2 in the reaction tube 10 is heated while the rare-earth magnet raw material 2 is heated.
To absorb hydrogen. With the hydrogen occlusion, the rare-earth magnet raw material 2 in the reaction tube 10 generates heat as described above. In this embodiment, the magnet raw material 2 for absorbing hydrogen was used.
Has a target temperature of about 800 ° C. and a storage time of about 3 hours. The target pressure of hydrogen is 1.2 to 1.5 atm.

In the hydrogen storage step according to the present embodiment, the second switching valve 56 is operated by the control device 98 to connect the second exhaust path 66 and the second concentrated path 71. In this state, the second vacuum pump 65 is operated by suction. As a result, the second exhaust passage 66, the second switching valve 56, the second concentrated passage 71,
The pressure in the dummy material holding tube 27 is reduced (for example, 10 ⁻⁵ to 10 ⁻⁹ Torr) through the second branch path 70, thereby forcibly removing the hydrogen occluded in the dummy material 25 of the dummy material holding tube 27. discharge. With such hydrogen release from the dummy material 25, the dummy material 25 absorbs heat.

That is, in the hydrogen storage step according to the present embodiment, the dummy material 25 is brought close to the rare earth magnet raw material 2 in the reaction tube 10 so as to be substantially synchronized with the heat generation action of the rare earth magnet raw material 2. At 25, an endothermic effect is generated. Therefore, the heat generation and the heat absorption are easily offset. Therefore, an increase in temperature due to the heat generation of the rare earth magnet raw material 2 in the reaction tube 10 in the hydrogen storage step is suppressed.

(Hydrogen release step) After the hydrogen occlusion step is completed as described above, a hydrogen release step is performed. That is, the control device 9
8, the first switching valve 52 is operated to operate the first concentrated path 3
1 and the first supply path 54 are not communicated, and the first concentrated path 31 and the first exhaust path 61 are communicated. In this state, the first vacuum pump 60 is operated by the control device 98 to reduce the pressure inside the reaction tube 10 to vacuum (for example, 10 ⁻⁵ to 10 ⁻⁹ Torr).
r). As a result, the hydrogen occluded in the rare earth magnet raw material 2 in the reaction tube 10 is forcibly released. With the release of hydrogen from the rare earth magnet raw material 2, the reaction tube 1
The rare-earth magnet raw material 2 within 0 absorbs heat.

The target temperature in such a hydrogen releasing step is 775 to 850 ° C., and the time is about 30 minutes. The hydrogen releasing process in each reaction tube 10 is performed uniformly. In the hydrogen releasing step according to the present embodiment, the second switching valve 56 is operated by the control device 98 so that the second exhaust path 66 and the second concentrated path 71 are not communicated with each other, and the second supply path 58
And the second concentrated route 71. Thereby, the hydrogen gas of the hydrogen gas supply device 5 is supplied to each dummy material holding pipe 27 via the second supply path 58, the second switching valve 56, the second concentration path 71, and the second branch path 70. You. Thereby, the dummy material 25 in each dummy material holding tube 27 absorbs hydrogen and generates heat.

That is, in the hydrogen releasing step according to the present embodiment, the dummy material 25 is added to the rare earth magnet raw material 2 in the reaction tube 10.
Are generated in the dummy material 25 so as to be substantially synchronized with the endothermic action of the rare-earth-based magnet raw material 2 in a state where are brought close to each other. Therefore, heat absorption and heat generation are easily offset. Therefore, the temperature drop due to the endothermic effect of the rare earth magnet raw material 2 in the reaction tube 10 in the hydrogen releasing step is suppressed.

After the hydrogen release process is completed, a quenching step of quenching the rare earth magnet raw material 2 is performed. The quenching step is performed by bringing cooling gas such as argon gas or cooling water into contact with the rare earth magnet raw material 2. The cooling gas or cooling water may be brought into contact with the reaction tube 10 for cooling. In this way, a rare earth magnet powder having improved magnetic properties is produced. (Effects) As described above, in the present embodiment, in the hydrogen storage step, an endothermic action is generated in the dummy material 25 so as to be substantially synchronized with the exothermic action of the rare-earth magnet raw material 2 in the reaction tube 10. Here, the rare earth magnet raw material 2 in the reaction tube 10
Since the dummy material 25 and the dummy material 25 are arranged close to each other, the heat generated by the rare earth magnet raw material and the heat absorbed by the dummy material 25 are easily offset. Therefore, the reaction tube 1 in the hydrogen storage step
The temperature rise due to the heat generation of the rare earth magnet raw material 2 within 0 can be suppressed.

Similarly, in the hydrogen releasing step, the reaction tube 1
0 so as to be substantially synchronized with the endothermic action of the rare earth magnet raw material 2,
The dummy material 25 generates heat. Therefore, the heat absorption of the rare earth magnet raw material 2 and the heat generation of the dummy material 25 are likely to be offset. Therefore, the reaction tube 10 in the hydrogen releasing step
The temperature drop due to the endothermic absorption of the rare-earth-based magnet raw material 2 therein is suppressed.

That is, in this embodiment, even if the rare earth magnet raw material 2 generates heat in the hydrogen absorbing step, the rare earth magnet raw material 2
Temperature can be made uniform and stable. Similarly, even in the hydrogen release step, even if the rare earth magnet raw material 2 absorbs heat, the temperature of the rare earth magnet raw material 2 can be made uniform and stable. Therefore, local variations in the magnetic properties of the manufactured rare-earth magnet powder can be avoided, and the rare-earth magnet powder manufactured in this example has the magnetic properties (maximum magnetic energy product, residual magnetic flux density,
Coercive force). Therefore, it is possible to contribute to high quality of the rare earth magnet powder, and it is suitable for mass production and industrialization of the rare earth magnet powder.

Further, in this embodiment, as described above, the rare-earth magnet raw material 2 to be subjected to the hydrogen treatment is divided and held in a small number of the reaction tubes 10 by small amounts, and the dummy material holding tubes 27 are provided in each reaction tube 10. The temperature fluctuation of the rare earth magnet raw material 2 can be suppressed for each of the reaction tubes 10. Therefore, excessive heat generation and excessive heat absorption of the rare-earth magnet raw material 2 in the reaction tube 10 are suppressed, which is more advantageous for suppressing temperature fluctuation, and more suitable for mass production and industrialization.

Further, in this embodiment, the amount of the rare earth magnet raw material 2 in the reaction tube 10 and the amount of the dummy material 2 in the dummy material holding tube 27 are changed.
The amount of 5 corresponds to the specific amount. Therefore, the degree of heat generation of the rare earth magnet raw material 2 in the reaction tube 10 and the degree of heat absorption of the dummy material 25 are basically easily compatible. Therefore, it is more advantageous to suppress the fluctuation of the temperature of the rare earth magnet raw material 2 in the reaction tube 10 in the hydrogen storage step.

In addition, in this embodiment, the rare-earth magnet raw material 2 divided in the reaction tube 10 is separated little by little and separated from each other. Therefore, the rare earth magnet raw material 2 in the reaction tube 10
Is less likely to affect the rare-earth magnet raw material 2 in the adjacent reaction tube 10. Therefore, local excessive heat generation or excessive heat absorption can be suppressed, which is more advantageous for uniformizing and stabilizing the temperature of the rare earth magnet raw material 2.

(Heat History Form) FIG. 3 schematically shows a heat history form of the rare earth magnet raw material 2 according to the above-described embodiment.
In this example, as described above, the rare earth magnet raw material 2 is 250
After occlusion of hydrogen at ° C, hydrogen is released and pre-treated, changing from a lump form to a granular form. As described above, the hydrogen storage step and the hydrogen release step are sequentially performed in the region near 800 ° C. by using the rare earth magnet raw material 2 in the form of powder or granules by the preliminary treatment.

After preliminarily treating the rare-earth magnet raw material 2 at 250 ° C., it is once cooled to a normal temperature range, and then cooled again to 80 ° C.
The hydrogen storage step and the hydrogen release step may be performed in a region near 0 ° C. (Heat treatment apparatus) A part of the manufacturing apparatus of the embodiment can be regarded as the heat treatment apparatus of the present invention. The components of the heat treatment apparatus include a heating device 4 and a temperature control device 45 which form a heating chamber 40 and incorporate heating means, a dummy material holding tube 27 which holds a dummy material 25, and a dummy material holding tube 27. A large number of loaded second branch paths 70
, A second branching device 7 composed of a second concentrating path 71 connecting the second branching paths 70, a hydrogen cylinder 50, a purifier 51, a second switching valve 56, and a second supply path 58. A second branching device 7 having a vacuum pump 65 and a second exhaust passage 66, and a control device 98.
Consists of

Here, the heating device 4 and the temperature control device 4
5 constitutes a heating vessel and a heating means of the heat treatment apparatus of the present invention. Similarly, the dummy material 25 and the dummy material holding tube 27 constitute a hydrogen storage alloy and a sealed container of the heat treatment apparatus of the present invention. Similarly, the second branching device 7, the exhaust device 6, and the control device 98 constitute a temperature control means of the heat treatment apparatus of the present invention.

This heat treatment device controls the temperature of the heating chamber 40 of the heating device 4 to a predetermined temperature by controlling the temperature of the temperature control device 45. Further, the inside of the heating chamber 40 is cooled or heated by the dummy material holding pipe 27 which absorbs and generates heat by controlling the hydrogen partial pressure by controlling the hydrogen partial pressure by the hydrogen cylinder 50, the exhaust device 6 and the control device 98. In this heat treatment apparatus, the temperature in the heating chamber can be controlled more accurately by the temperature control means disposed in the heating chamber 40.

In this embodiment, a plurality of dummy material holding tubes 27 are employed as a closed container, but one dummy material holding tube 27 may be used. Further, as the heating device, a heating furnace such as a normal electric furnace or a Tamman tube furnace can be used.

[Brief description of drawings]

FIG. 1 is a configuration diagram illustrating the concept of an apparatus according to an embodiment.

FIG. 2 is an enlarged configuration diagram showing the vicinity of a reaction tube.

FIG. 3 is a graph showing a thermal history form of a rare earth magnet raw material.

[Explanation of symbols]

In the figure, 1 is a raw material holding unit, 10 is a reaction tube, 2 is a rare earth magnet raw material, 25 is a dummy material, 27 is a dummy material holding tube,
4 is a heating device, 40 is a heating chamber, 45 is a temperature control device, 5
Denotes a hydrogen gas supply device, 6 denotes an exhaust device, 60 and 65 denote vacuum pumps, and 98 denotes a control device.

Claims (8)

[Claims] 1. A raw material holding portion for holding a rare earth magnet raw material having a characteristic that magnetic characteristics are improved by absorbing hydrogen with heat generation and releasing hydrogen with heat absorption, and a rare earth magnet raw material of the raw material holding portion. A heating device for heating, a hydrogen gas feeding device for feeding hydrogen to the raw material holding part to occlude hydrogen in the rare earth magnet raw material of the raw material holding part, and reducing the raw material holding part to reduce the raw material holding part An exhaust device for releasing hydrogen from the rare earth-based magnet raw material of,
A heat functional material holding portion for holding a heat functional material having endothermic and heat generating properties; and a heat absorbing material for the heat functional material, substantially in synchronization with heat generation of the rare earth magnet raw material of the raw material holding portion, and An apparatus for producing a rare earth magnet powder, comprising: a synchronizing means for generating heat from the thermal functional material substantially in synchronization with heat absorption of the rare earth magnet raw material. 2. The apparatus for producing rare earth magnet powder according to claim 5, wherein the raw material holding portion is composed of an appropriate number of tubes for dividing and holding the rare earth magnet raw material. 3. The same number of thermal function material holding portions as the tubular body are provided,
The apparatus for manufacturing a rare earth magnet powder according to claim 6, wherein each of the thermal functional material holding units is provided inside each of the tubes. 4. The apparatus for producing rare earth magnet powder according to claim 5, wherein the thermal functional material is a dummy material containing a rare earth magnet of the same type as the rare earth magnet raw material as a main component. 5. A heating container forming a heating chamber, heating means for heating the heating chamber, a closed container arranged in the heating chamber for heating or cooling the heating chamber, and hydrogen arranged in the closed container. A heat treatment device comprising: a temperature control means comprising a storage alloy and a hydrogen gas pressure control device for controlling the hydrogen gas pressure in the closed container. 6. The heat treatment apparatus according to claim 9, wherein the heating container is a cylindrical first pipe, and the closed container is a second pipe arranged in the first pipe. 7. The heating means is a heating furnace having a storage chamber therein, and a heating portion inside or on an inner peripheral surface of a furnace wall forming the storage chamber, wherein the heating container is a storage chamber of the heating furnace. The heat treatment apparatus according to claim 10, which is provided in the. 8. The heat treatment apparatus according to claim 11, wherein a plurality of the heating containers are housed in the housing chamber of the heating furnace.