JP2012234895A - Method of manufacturing r-t-b based sintered magnet - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method of manufacturing an R-T-B based sintered magnet which can reduce occurrence of deposition between an R-T-B based sintered magnet and a support body, and also achieves an efficient supply of a heavy rare earth element RH from RH supply sources to R-T-B based sintered magnet bodies.SOLUTION: A vertical multi-stage arrangement of RH supply sources and R-T-B based sintered magnet bodies is obtained by respectively interposing a spacer having a specific shape therebetween. This achieves a considerable reduction of the occurrence of deposition between an R-T-B based sintered magnet and a support body than using a conventionally employed support body, such as a mesh. Additionally, a small contact area between the RH supply source and the R-T-B based sintered magnet body allows an efficient supply of a heavy rare earth element RH from the RH supply sources to the R-T-B based sintered magnet bodies, thereby improving a yield of the heavy rare earth element RH.

Description

  The present invention relates to a method for producing an RTB-based sintered magnet.

  R-T-B based sintered magnets (R is at least one of rare earth elements, T is Fe or Fe and Co) are known as the most powerful magnets among permanent magnets, It is used in various motors for electric vehicles and home appliances.

However, the _RTB -based sintered magnet has a _reduced coercive force H _cJ (hereinafter simply referred to as “H _cJ ”) at a high temperature, causing irreversible thermal demagnetization. Therefore, especially when used for a motor for a hybrid vehicle or an electric vehicle, it is required to maintain a high _HcJ even at a high temperature.

In recent years, for the purpose of improving _{HcJ of RTB} -based sintered magnets, after sintering, heavy rare earth elements RH such as Dy, Ho, Tb, etc., are supplied to the magnet surface using vapor deposition means, and the heavy rare earth elements There has been proposed a vapor deposition diffusion method that improves H _cJ while suppressing a decrease in residual magnetic flux density B _r (hereinafter simply referred to as “B _r ”) by diffusing RH into the magnet.

  Patent Document 1 discloses that an R-T-B sintered magnet and a bulk body containing a heavy rare earth element RH are arranged to face each other at a predetermined interval, and these are heated to a predetermined temperature. The vapor deposition diffusion method is disclosed in which the heavy rare earth element RH is diffused into the inside of the RTB-based sintered magnet while supplying the rare earth element RH to the surface of the RTB-based sintered magnet.

  In Patent Document 1, as a method of performing simultaneous vapor diffusion from both sides of an RTB-based sintered magnet, an RTB-based sintered magnet is placed on an Nb net, and a predetermined interval is formed above and below it. A method of disposing the bulk body containing the heavy rare earth element RH is disclosed.

  Patent Document 2 discloses that a metal evaporation material containing at least one of Dy and Tb and an R-T-B system sintered magnet are housed in a processing box and heated to a predetermined temperature in a vacuum atmosphere. An evaporation diffusion method is disclosed in which it is evaporated and attached to an R-T-B system sintered magnet, and the attached Dy and Tb metal atoms are diffused to the surface of the sintered magnet and / or to the grain boundary phase. .

  In Patent Document 2, the metal evaporation material and the R-T-B system sintered magnet are not in contact with each other, and the evaporated metal atoms are allowed to pass through. A storage method is disclosed in which an expanded metal in which a plurality of sintered magnets can be juxtaposed is interposed, and a metal evaporation material and an RTB-based sintered magnet are alternately stacked in the vertical direction.

International Publication No. 2007/102391 JP 2009-135393 A

  In the vapor deposition diffusion method described in Patent Documents 1 and 2, a concentrated layer of heavy rare earth element RH is formed in the main phase outer shell portion of the RTB-based sintered magnet using a diffusion reaction by heat treatment. At that time, the heavy rare earth element RH diffuses from the surface of the RTB-based sintered magnet into the RTB-based sintered magnet, and at the same time, into the RTB-based sintered magnet. A liquid phase component mainly composed of contained light rare earth element RL (RL is at least one of Nd and Pr) diffuses toward the surface of the RTB-based sintered magnet. In this way, the heavy rare earth element RH passes from the surface of the RTB-based sintered magnet to the inside, and the light rare earth element RL extends from the interior of the RTB-based sintered magnet to the surface. Due to mutual diffusion, an elution portion mainly composed of the light rare earth element RL is formed on the surface of the RTB-based sintered magnet. This elution part reacts with the support body which supports the R-T-B system sintered magnet. Therefore, the support and the RTB-based sintered magnet are fixed (hereinafter referred to as “welding”).

  In Patent Documents 1 and 2, an RH diffusion source (corresponding to a metal evaporation material in Patent Document 2) and an RTB-based sintered magnet are interposed as a support with an Nb net or an expanded metal, and RH diffusion is performed. Sources and RTB-based sintered magnets are alternately stacked in the vertical direction. The Nb net and the expanded metal need strength to support the RH diffusion source and the RTB-based sintered magnet. For this reason, there is a limit to increasing the aperture ratio of the Nb net or the expanded metal. For example, Patent Document 2 describes that the opening ratio of the expanded metal may be 30% to 80%, and as an example, describes the case where the expanded metal is formed with an opening ratio of about 60%. As described above, since the opening ratio of the support such as the Nb net or the expanded metal is limited, the contact area with the RTB-based sintered magnet is increased. Therefore, when a plurality of RTB-based sintered magnets are processed by the vapor deposition diffusion method, many RTB-based sintered magnets are welded to a support such as an Nb net or an expanded metal. was there.

  If the R-T-B system sintered magnet that causes welding is forcibly removed from the support, the R-T-B system sintered magnet itself may be destroyed. Therefore, it is necessary to remove carefully, and the man-hour of the removal work of a support body and a RTB system sintered magnet will increase. Therefore, it is desired to reduce the contact area between the support and the RTB-based sintered magnet as much as possible to reduce the welding between the support and the RTB-based sintered magnet.

  Further, as in Patent Documents 1 and 2, when the contact area between the support and the RTB-based sintered magnet is large, the heavy rare earth element RH supplied from the RH diffusion source is converted into the support (Nb network or A large amount of the rare earth element RH is wasted. Therefore, in order to supply the heavy rare earth element RH from the RH diffusion source to the RTB-based sintered magnet with a high yield, the contact area between the support and the RTB-based sintered magnet can be reduced. It is desired.

  The present invention has been made to solve the above-mentioned problems, and the object of the present invention is to reduce the occurrence of welding between the R-T-B system sintered magnet and the support, and from the RH supply source. An object of the present invention is to provide a method for producing an RTB-based sintered magnet that can efficiently supply the heavy rare earth element RH to the RTB-based sintered magnet.

  According to the first aspect of the present invention, there is provided a method of manufacturing an RTB-based sintered magnet according to an embodiment of the present invention, wherein an RTB-based sintered magnet body (where R is at least one rare earth element, T is Fe or Fe and Co) and an RH source (a metal comprising heavy rare earth element RH or an alloy containing 25 atomic% or more of heavy rare earth element RH, where heavy rare earth element RH is at least one of Dy, Ho, and Tb) The heavy rare earth element RH is supplied from the RH supply source to the surface of the RTB-based sintered magnet body by heating in a state of being arranged in multiple stages in the vertical direction via a spacer. In the vapor deposition diffusion process in which the element RH is diffused into the RTB-based sintered magnet body, the spacer includes a plurality of rod-like members and / or small piece-like members having a thickness of 0.1 mm to 15 mm. The contact area of the spacer to the RTB-based sintered magnet body is 15% or less of the total area of the RTB-based sintered magnet body on the side in contact with the spacer, and the The contact area of the spacer with the RH supply source is 15% or less of the total area of the RH supply source on the side in contact with the spacer.

  According to a second aspect of the present invention, in the method for producing an RTB-based sintered magnet according to the first aspect, the spacer may be the RTB-based sintered magnet body and the RH supply source. Two or more are arranged in a region of ¼ of the dimension in the width direction from both ends in each width direction and / or in a region of ¼ in the length direction from both ends in each length direction.

  According to a third aspect of the present invention, in the method for producing an RTB-based sintered magnet according to the first or second aspect, the RTB-based sintered magnet body and the RH supply source are The vapor deposition diffusion treatment is performed by heating to 800 ° C. or more and 950 ° C. or less.

  According to a fourth aspect of the present invention, in the method for manufacturing an RTB-based sintered magnet according to the third aspect, the vapor deposition diffusion treatment is performed by setting the pressure in the processing case to 0.1 Pa to 50 Pa. It is characterized by that.

  According to a fifth aspect of the present invention, in the method for producing an RTB-based sintered magnet according to the third or fourth aspect, after the vapor deposition diffusion treatment, the pressure in the treatment case is set to a pressure of 200 Pa or more and 2 kPa. In the following, heat treatment is performed by heating the RTB-based sintered magnet body and the RH supply source to 800 ° C. or more and 950 ° C. or less.

  In the present invention, the RTB-based sintered magnet before the vapor deposition diffusion treatment is referred to as an “RTB-based sintered magnet body”, and the RTB-based sintered magnet after the vapor deposition diffusion treatment is used. Are referred to as “R-T-B system sintered magnet”.

  According to the present invention, an RH supply source and an RTB-based sintered magnet can be obtained by using a spacer having a specific shape instead of a support such as Nb net and expanded metal used in Patent Documents 1 and 2. The contact area with the body can be greatly reduced. Therefore, generation | occurrence | production of welding with a RTB system sintered magnet and a spacer can be reduced, and the removal man-hour with an RTB system sintered magnet can be reduced significantly. Further, since the contact area is small, the heavy rare earth element RH can be efficiently supplied from the RH supply source to the RTB-based sintered magnet body, and the yield of the heavy rare earth element RH can be improved.

It is explanatory drawing which shows an example of embodiment of this invention. It is explanatory drawing which shows the arrangement | positioning area | region of a spacer. It is explanatory drawing which shows the arrangement | positioning area | region of a spacer. It is explanatory drawing which shows the arrangement | positioning area | region of a spacer. It is explanatory drawing which shows an example which has arrange | positioned the rod-shaped member. It is explanatory drawing which shows an example which has arrange | positioned the rod-shaped member. It is explanatory drawing which shows an example which has arrange | positioned the small piece member. It is explanatory drawing which shows an example arrange | positioned combining the rod-shaped member and the small piece-shaped member.

In the present invention, the contact area between the spacer and the R-T-B system sintered magnet body refers to the R-T-B system on the side in contact with the spacer in the individual rod-like member or small piece member constituting the spacer. It is defined as the sum of the maximum areas in the cross section parallel to the surface of the sintered magnet body. For example, an R-T-B system sintered magnet body having a total area of 1000 mm ² (width 20 mm x length 50 mm) on the side in contact with the spacer is circular in cross section (longitudinal section) 3 mm in diameter x 25 mm in length. When two spacers made of rod-shaped members are arranged so that the peripheral surfaces are in contact with each other, the maximum area of the cross-section of the rod-shaped member having a circular cross section parallel to the surface of the RTB-based sintered magnet body is: Cross section passing through the center of the circle, that is, diameter × length. In this case, the contact area is 150 mm ² (3 mm × 25 mm × 2) / 1000 mm ² (20 mm × 50 mm) × 100% = 15%.

  When the cross section (longitudinal cross section) is a rod-shaped member or a small piece member such as a triangle or trapezoid, the maximum area of the cross section parallel to the surface of the RTB-based sintered magnet body is a triangle. If it is a trapezoid, the longest base x length. In the above description, the contact area between the spacer and the RTB-based sintered magnet body has been described, but the contact area between the spacer and the RH supply source is the same.

  When the vertical cross-sectional shape of the spacer is circular, since the spacer is in line contact with the RH supply source and the RTB-based sintered magnet body, the actual contact area is smaller than the contact area defined above. . Therefore, in the present invention, when the contact area between the spacer and the RH supply source or the R-T-B system sintered magnet body is the same, the vertical cross-sectional shape of the spacer is more than the multi-sided shape in surface contact. A circular shape that is in line contact is preferable because the actual contact area is small.

The vapor deposition diffusion treatment in the present invention means that the R—T—B system sintered magnet body and the RH supply source are heated, whereby the heavy rare earth element RH is transferred from the RH supply source to the surface of the R—T—B system sintered magnet body. while supplying to, by diffusing the heavy rare-earth element RH inside of the R-T-B sintered magnet body while suppressing a decrease in B _r, and improves the H _cJ.

  When using a support such as an Nb net or expanded metal as described in Patent Documents 1 and 2, strength to support the RTB-based sintered magnet body or RH diffusion source is required. there were. For this reason, there is a limit to increasing the aperture ratio of the Nb net or the expanded metal. In general, the opening ratio of Nb nets and expanded metals provided on the market is usually about 60%, and about 80% at the maximum. That is, the contact area of the support is usually about 40% of the total area on the side in contact with the RTB-based sintered magnet body or the support of the RH supply source, and is about 20% at the minimum. On the other hand, the spacer having a specific shape in the present invention can support the RTB-based sintered magnet body and the RH supply source with a small contact area. In order to achieve the object of the present invention, the contact area of the spacer needs to be 15% or less of the total area on the side in contact with the RTB-based sintered magnet body or the spacer of the RH supply source. Preferably, the contact area is 10% or less, more preferably 5% or less.

  As described above, by using the spacer in the present invention, the contact area between the spacer, the RTB-based sintered magnet body, and the RH supply source can be reduced as compared with the case of using a support such as an Nb net or expanded metal. It can be greatly reduced. Therefore, it is possible to reduce the occurrence of welding with the RTB-based sintered magnet, and to efficiently supply the heavy rare earth element RH from the RH supply source to the RTB-based sintered magnet body. The yield of heavy rare earth element RH (the difference in the weight of the RH supply source before and after the treatment and the weight of the heavy rare earth element RH diffused in the magnet in the R-T-B sintered magnet after the treatment (component It is possible to improve the ratio) to the measurement result by analysis).

  EMBODIMENT OF THE INVENTION Below, the form for implementing this invention is demonstrated based on drawing. In the drawings, the same parts are denoted by the same reference numerals.

  FIG. 1 is an explanatory view showing an example of an embodiment of the present invention in which an RH supply source 2 and an RTB-based sintered magnet body 3 are arranged in multiple stages in the vertical direction with spacers 4 in a processing case 1. It is. As shown in FIG. 1, an RH supply source 2 is arranged on the bottom of the processing case 1, and a spacer 4 made of two rod-like members is arranged on the RH supply source 2. The RTB-based sintered magnet body 3 is disposed on the spacer 4, and the spacer 4 is disposed on the RTB-based sintered magnet body 3. In this way, the RH supply source 2 and the R-T-B system sintered magnet bodies 3 are alternately arranged in multiple stages in the vertical direction via the spacers 4.

  If the spacer 4 can stably arrange the RH supply source 2 and the RTB-based sintered magnet body 3 in multiple stages alternately in the vertical direction, the arrangement position is not particularly limited. For example, two rod-like members may be arranged at arbitrary positions, or a plurality of small piece-like members may be scattered at arbitrary positions. As a preferred embodiment, the spacer is formed by using the RTB-based sintered magnet body and the RH supply source from both ends in the width direction to a quarter region of the dimension in the width direction and / or both ends in the length direction. It is preferable to arrange two or more in a region of ¼ of the dimension in the length direction. This will be described in detail below.

  2-4 is explanatory drawing which shows the arrangement | positioning area | region of a spacer as a preferable form. In FIG. 2, four small pieces are provided in a region 5 (shaded portion) of 1/4 (1/4 W in the drawing) of the width direction from both ends in the width direction W of the RTB-based sintered magnet body 3. A spacer 4 made of a member is disposed. Further, in FIG. 3, the region 2 (shaded part) is ¼ (¼L in the figure) of the dimension in the length direction from both ends in the length direction L of the RTB-based sintered magnet body 3. A spacer 4 made of a small piece-like member is arranged. Further, in FIG. 4, spacers 4 made up of three small pieces are arranged in a region 5 (shaded portion) obtained by combining FIGS. 2 and 3. As described above, the RH supply source 2 is more stable when the two or more spacers 4 are arranged at both ends in the length direction or the width direction rather than the center portion of the RTB-based sintered magnet body 3. And RTB-based sintered magnet bodies 3 can be arranged in multiple stages alternately in the vertical direction.

  The processing case 1 and the spacer 4 are deformed or altered during vapor deposition diffusion processing, such as refractory metals such as Mo, W, Ta, and ceramic materials including boron nitride, zirconia, alumina, yttria, calcia, magnesia, etc. It is preferable to use a difficult material. Further, an oxide such as zirconia, alumina or yttria may be sprayed on the surface of a refractory metal such as Mo.

  The spacer 4 is selected so that the contact area is 15% or less according to the size of the RH supply source 2 and the RTB-based sintered magnet body 3. The thickness of the spacer 4 is preferably set in the range of 0.1 mm to 15 mm. If the distance between the RH supply source 2 and the R-T-B system sintered magnet body 3 is too short, the two come into contact with each other due to dimensional variations of the RH supply source 2 and the R-T-B system sintered magnet body 3. There is a possibility. Therefore, the thickness of the spacer 4 is preferably 0.1 mm or more. Moreover, by setting it as 15 mm or less, the heavy rare earth element RH can be efficiently supplied to the RTB-based sintered magnet body 3.

  In FIG. 1, the spacer 4 uses a rod-shaped member, but a small piece-like member or the like can also be used. These spacers are preferably selected according to the shape and size of the RH supply source 2 and the RTB-based sintered magnet body 3. Hereinafter, the rod-shaped member and the small piece-shaped member will be described in detail.

  The rod-shaped member may be arranged in a direction parallel to the contact surface with the RH supply source 2 or the RTB-based sintered magnet body 3 in the length direction, and the cross-sectional (vertical cross-sectional) shape is arbitrary. The RH supply source 2 and the RTB-based sintered magnet body 3 may be in surface contact, but line contact is preferable. For example, the cross-sectional shape is preferably circular or elliptical.

  In FIG. 5, two rod-like members 4 a are arranged in parallel to both end portions of the RH supply source 2 and the RTB-based sintered magnet body 3. However, it is not particularly necessary to strictly manage the angle and direction, and they may be arranged obliquely. When the RH supply source 2 and the RTB-based sintered magnet body 3 are arranged in multiple stages, the rod-like member 4a may be arranged so as not to become unstable when arranged obliquely. Further, the rod-like member 4a may be curved at both ends to prevent rolling.

  As shown in FIG. 6, four rod-shaped members 4a may be combined into a frame shape, or four may be connected and used as an integrated product.

  FIG. 7 is a plan view showing an example in which small pieces 4b are arranged. In FIG. 7, cylindrical small pieces 4 b are arranged at four corners on the RTB-based sintered magnet body 3. If the RH supply source 2 and the R-T-B system sintered magnet body 3 can be stably arranged in multiple stages in the vertical direction, the small piece-like member 4b can have the RH supply source 2 and the R-T-B system sintered magnet body 3. The location and the shape thereof are arbitrary. For example, a substantially spherical shape made of a polyhedron may be scattered at several locations on the RH supply source 2 and the R-T-B system sintered magnet body 3. Further, it may be a dice shape other than a substantially spherical shape made of a polyhedron, a conical shape, or a rectangular shape.

  FIG. 8 is a plan view showing an example in which the rod-like member 4a and the small piece-like member 4b are arranged in combination on the RTB-based sintered magnet body. As shown in FIG. 8, the rod-shaped member 4 a is disposed at both ends of the RTB-based sintered magnet body 3, and the small piece-like member 4 b is positioned at the substantially central position of the RTB-based sintered magnet body 3. You may arrange.

  As described above, by using a spacer made of a plurality of rod-like members and / or small piece-like members, the contact area can be reduced as compared with the case of using a support such as an Nb net or an expanded metal. .

The RH supply source 2 is a metal composed of a heavy rare earth element RH or an alloy containing 25 atomic% or more of the heavy rare earth element RH, and the heavy rare earth element RH is at least one of Dy, Ho, and Tb. For example, Dy metal, Tb metal, Ho metal, DyFe alloy, TbFe alloy, and HoFe alloy. Other elements may be included in addition to Dy, Tb, Ho, and Fe. The size of the RH supply source 2 is not particularly limited, such as a block shape (bulk body) or a plate shape, but it is preferable that the RH supply source 2 contains 25 atomic% or more of the heavy rare earth element RH. When the content of the heavy rare earth element RH is less than 25 atomic%, the supply amount of the heavy rare earth element RH from the RH supply source 2 is decreased, and the processing time is very long in order to obtain the desired effect of improving _HcJ. Therefore, it is not preferable.

  The processing conditions for performing the vapor deposition diffusion processing may be performed by a known method. An example of a preferred method is described in detail below.

  First, the RH supply source 2 and the RTB-based sintered magnet body 3 are alternately arranged in multiple stages in the vertical direction via the spacers 4 in the processing case 1, and the processing case 1 is placed in the vapor deposition diffusion processing apparatus ( (Not shown). Thereafter, the RH supply source 2 and the RTB-based sintered magnet body 3 are heated to 800 ° C. or higher and 950 ° C. or lower to perform vapor deposition diffusion treatment. If the temperature is lower than 800 ° C., insufficient supply of heavy rare earth element RH to the R—T—B based sintered magnet body 3 may occur. If the temperature exceeds 950 ° C., the heavy rare earth element RH is excessively supplied to the RTB-based sintered magnet body 3, which may increase the number of welded portions with the spacer.

  In addition, in the said vapor deposition diffusion process, it is preferable that the atmospheric pressure in the process case 1 shall be 0.1 Pa or more and 50 Pa or less. When the vapor deposition diffusion treatment is performed at an atmospheric pressure of less than 0.1 Pa, the heavy rare earth element RH may be excessively supplied, and the number of welded portions between the RTB-based sintered magnet 3 and the spacer 4 increases. There is a risk that. On the other hand, when the pressure exceeds 50 Pa, there is a possibility that the supply of the heavy rare earth element RH to the RTB-based sintered magnet body 3 cannot be sufficiently ensured.

  After the vapor deposition diffusion treatment, it is preferable to further perform a heat treatment by heating the atmospheric pressure in the treatment case 1 to 200 Pa to 2 kPa, heating the RH supply source and the RTB-based sintered magnet to 800 ° C. to 950 ° C. . By setting the atmospheric pressure to 200 Pa or more and 2 kPa or less, the heavy rare earth element RH is not supplied from the RH supply source 2 to the surface of the RTB-based sintered magnet body 3, and only diffusion proceeds. Further, by setting the temperature range to 800 ° C. or more and 950 ° C. or less, the heavy rare earth element RH can be more uniformly diffused into the RTB-based sintered magnet.

  When the vapor deposition diffusion treatment apparatus for performing the vapor deposition diffusion treatment is composed of a single processing chamber, and when the heat treatment is continued in the processing chamber, an inert gas is flowed to adjust the atmospheric pressure to 200 Pa or more and 2 kPa or less. Then, the heat treatment may be performed.

  When the vapor deposition diffusion treatment apparatus that performs the vapor deposition diffusion treatment includes two treatment chambers, that is, a treatment chamber that performs the vapor deposition diffusion treatment and a treatment chamber that performs the heat treatment, the treatment chamber in which the heat treatment is performed is 200 Pa or more and 2 kPa or less. A processing temperature of 800 ° C. or higher and 950 ° C. or lower is set in advance at an atmospheric pressure, and after performing the vapor deposition diffusion treatment in the vapor deposition diffusion treatment chamber, the processing case 1 is transferred to the treatment chamber in which the heat treatment is performed. The heat treatment may be performed by carrying it on a table (not shown).

  The heat treatment is not necessarily performed by the same apparatus as the vapor deposition diffusion processing apparatus, and may be performed by another apparatus.

It is preferable to subject the RTB-based sintered magnet after the vapor deposition diffusion treatment to a surface treatment. The surface treatment may be a known surface treatment, and for example, a surface treatment such as Al vapor deposition, electric Ni plating, or resin coating can be performed. Prior to the surface treatment, a known pretreatment such as sandblasting, barrel treatment, or mechanical polishing may be performed. Moreover, you may perform the process grinding | polishing for a dimension adjustment. The polishing amount for adjusting the dimensions is 1 to 300 μm, preferably 5 to 100 μm, and more preferably 10 to 30 μm. Even after these surface treatment and processing / polishing steps, the _HcJ improvement effect is hardly changed.

  In all the following experiments, in order to perform the vapor deposition diffusion treatment, first, the RH supply source 2 is disposed on the bottom in the treatment case 1. Next, the spacer 4 is disposed on the RH supply source 2, and the RTB-based sintered magnet body 3 is disposed thereon. Thus, the RH supply source 2 and the RTB-based sintered magnet body 3 are alternately arranged in multiple stages in the vertical direction via the spacers. The treatment case 1 for use in the experiment was prepared with a size of height 430 × width 420 × length 520 (mm).

[Example 1]
R-T-B system sintering whose composition is Nd _19.3 Pr _5.7 Dy _4.3 B _0.95 Co _2.0 Al _0.15 Cu _0.1 Ga _0.08 balance Fe (mass%) Magnet body 3 was prepared. The magnetic properties were B _r = 1.31 T and H _cJ = 1740 kA / m.

  The RTB-based sintered magnet body 3 was processed into a thickness of 20 × width of 65 × length of 90 (mm). The RH supply source 2 was also prepared with Dy metal having substantially the same dimensions as the processed RTB sintered magnet body 3. Moreover, the spacer 4 prepared the rod-shaped member 4a with a circular cross section. The rod-shaped member 4a had an outer diameter of 3 mm and a length of 60 mm.

  As shown in FIG. 5, the RH supply source 2 and the RTB-based sintered magnet bodies 3 are alternately arranged in multiple stages in the vertical direction through the spacer 4 in which the rod-like member 4 a is arranged in the processing case 1.

After raising the temperature in the treatment case 1 of the present invention to 900 ° C., vapor deposition diffusion treatment was performed in a vacuum at a pressure of 10 ⁻³ Pa for 2 hours. After the vapor deposition diffusion treatment, heat treatment was further performed at 900 ° C. and a pressure of 1.5 kPa for 6 hours to produce an R-T-B system sintered magnet.

[Example 2]
The RTB-based sintered magnet body 3 having the same composition and magnetic characteristics as in Example 1 was processed into a thickness of 20 × width of 130 × length of 210 (mm). The RH supply source 2 was also prepared with Dy metal having substantially the same dimensions as the processed RTB sintered magnet body 3. Moreover, the spacer 4 prepared the rod-shaped member 4a with a circular cross section. There were two types of circular outer diameters of φ5 mm × 110 mm and φ5 × 200 mm.

  As shown in FIG. 6, the RH supply source 2 and the RTB-based sintered magnet body 3 are alternately multi-staged in the vertical direction through the spacer 4 in which the rod-like members 4 a are arranged in a frame shape in the processing case 1. Then, the same vapor deposition diffusion treatment as in Example 1 was performed, and an RTB-based sintered magnet was produced.

Example 3
The RTB-based sintered magnet body 3 having the same composition and magnetic characteristics as in Example 1 was processed into a thickness of 20 × width of 110 × length of 110 (mm). The RH supply source 2 was also prepared with Dy metal having substantially the same dimensions as the processed RTB sintered magnet body 3. Moreover, the spacer 4 prepared the cylindrical small piece member 4b. The outer diameter was 4 mm and the thickness was 5 mm.

  As shown in FIG. 7, the RH supply source 2 and the RTB-based sintered magnet body 3 are alternately arranged in the vertical direction through spacers 4 in which small pieces 4 b are arranged at four corners in the processing case 1. And the same vapor deposition diffusion treatment as in Example 1 was performed to produce an RTB-based sintered magnet.

[Comparative Example 1]
An RTB-based sintered magnet was produced under the same conditions as in Example 1 except that a net (3 mesh, aperture ratio 56%) knitted with a 2 mm diameter wire rod was used instead of the spacer. .

Example 4
An RTB-based sintered magnet was produced under the same conditions as in Example 1 except that the atmospheric pressure of the vapor deposition diffusion treatment was 3.0 Pa.

The results of Examples 1 to 4 and Comparative Example 1 are shown in Table 1. In Table 1, “pressure” indicates an atmospheric pressure (pressure in the processing case) during the vapor deposition diffusion treatment. “ _{ΔH cJ} ” indicates the difference between H _cJ (1740 kA / m) of the _RTB -based sintered magnet body before processing and H _cJ after processing. "△ _{B r"} indicates the difference between the _{B r} after treatment with pretreatment the R-T-B-based sintered magnet body _B r (1.31T). “Welding rate” is the number of R-T-B system sintered magnets that were welded when the R-T-B system sintered magnet was removed from the spacer, By dividing by, the percentage of welding is shown in%. The “contact area” is obtained by dividing the contact area of the spacer by the total area of the RTB-based sintered magnet body on the side in contact with the spacer, thereby obtaining the RTB-based sintered magnet in the spacer contact area. The percentage of contact with the body is shown in%. “Dy yield” is calculated from the weight change before and after the vapor deposition diffusion treatment of the RTB-based sintered magnet and the RH supply source (Dy metal) (Dy increase amount of RTB-based sintered magnet) / (Dy This is a value calculated by (metal reduction amount) × 100%. “Number of treatments” indicates the number of R—T—B system sintered magnets used in each of Example 1, Example 2, Example 3, Example 4, and Comparative Example 1.

In Comparative Example 1, the R-T-B system sintered magnet was welded in a mesh shape. In all the examples, compared with Comparative Example 1, the welding rate was less than half, which was significantly reduced. Furthermore, the Dy yield was also improved as compared with Comparative Example 1.
Further, in Example 4, no welding between the RTB-based sintered magnet and the spacer was observed, and the Dy yield was significantly improved as compared with the comparative example.

  As mentioned above, according to the Example, generation | occurrence | production of the welding of a RTB system sintered magnet can be reduced significantly. Thereby, the removal man-hour after a vapor deposition diffusion process can be reduced significantly, and it becomes possible to perform the vapor deposition diffusion process suitable for mass production. In addition, since the contact area is small, it is possible to efficiently supply the heavy rare earth element RH from the RH supply source to the RTB-based sintered magnet, and it is possible to improve the yield of the heavy rare earth element RH.

  The RTB-based sintered magnet according to the present invention can be suitably used for various motors for hybrid vehicles, electric vehicles, home appliances, and the like.

DESCRIPTION OF SYMBOLS 1 Processing case 2 RH supply source 3 RTB system sintered magnet body 4 Spacer 4a Bar-shaped member 4b Small piece-like member

Claims (5)

In the processing case,
R-T-B system sintered magnet body (R is at least one of rare earth elements, T is Fe or Fe and Co),
RH supply source (a metal comprising heavy rare earth element RH or an alloy containing 25 atomic% or more of heavy rare earth element RH, where heavy rare earth element RH is at least one of Dy, Ho and Tb),
By heating in a multi-stage arrangement in the vertical direction through the spacer,
While supplying the heavy rare earth element RH from the RH supply source to the surface of the RTB-based sintered magnet body, the heavy rare earth element RH is diffused into the RTB-based sintered magnet body. In the vapor deposition diffusion process,
The spacer comprises a plurality of rod-like members and / or small piece-like members having a thickness of 0.1 mm to 15 mm,
The contact area of the spacer to the RTB-based sintered magnet body is as follows:
15% or less of the total area of the RTB-based sintered magnet body on the side in contact with the spacer, and
The contact area of the spacer to the RH supply source is
The manufacturing method of the RTB system sintered magnet characterized by being 15% or less of the total area of the RH supply source on the side in contact with the spacer.   The spacers are arranged in the length direction from both ends of each width direction of the RTB-based sintered magnet body and the RH supply source, and / or from both ends in the length direction. The method for producing an RTB-based sintered magnet according to claim 1, wherein two or more are arranged in an area of ¼ of the size of the sintered magnet.   3. The RT according to claim 1, wherein the deposition diffusion treatment is performed by heating the RTB-based sintered magnet body and the RH supply source to 800 ° C. or more and 950 ° C. or less. -Manufacturing method of B type sintered magnet.   The method for producing an R-T-B system sintered magnet according to claim 3, wherein the vapor deposition diffusion treatment is performed at a pressure in the treatment case of 0.1 Pa to 50 Pa.   After the vapor deposition diffusion treatment, the pressure in the treatment case is set to 200 Pa or more and 2 kPa or less, and the RTB-based sintered magnet and the RH supply source are heated to 800 ° C. or more and 950 ° C. or less to perform heat treatment. The manufacturing method of the RTB type | system | group sintered magnet of Claim 3 or 4 characterized by these.

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