Method for preparing rare earth sintered magnet
09711280 ยท 2017-07-18
Assignee
Inventors
- Eiji Uesaka (Echizen, JP)
- Osamu Kohno (Echizen, JP)
- Kenji Imamura (Echizen, JP)
- Yoshihiro Umebayashi (Echizen, JP)
- Takahiro Hashimoto (Echizen, JP)
Cpc classification
H01F41/0246
ELECTRICITY
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B30B11/008
PERFORMING OPERATIONS; TRANSPORTING
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B22F2003/033
PERFORMING OPERATIONS; TRANSPORTING
International classification
B22F3/03
PERFORMING OPERATIONS; TRANSPORTING
B22F1/00
PERFORMING OPERATIONS; TRANSPORTING
B30B11/00
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A rare earth sintered magnet is prepared from a corresponding alloy powder, using a mold comprising a die, an upper punch, and a lower punch which is divided into a plurality of punch segments which are independently movable within the die. The method comprises the steps of filling the mold cavity with the alloy powder when one or more selected punch segments are moved to a higher position than the remaining punch segments; moving the selected punch segments down to the position where the selected and remaining punch segments assume the normal shape of the lower punch during the compression step; compressing the alloy powder between the upper and lower punches under a magnetic field while the normal shape of the lower punch is maintained, for thereby molding a compact; and heat treating the compact.
Claims
1. A method for preparing a rare earth sintered magnet from a corresponding alloy powder using a mold, said mold comprising a die, an upper punch having a pressure surface, and a lower punch having a pressure surface, the pressure surface of one or both of the upper and lower punches being shaped non-planar, the lower punch being divided into a plurality of punch segments which are independently movable within the die in a compression direction, provided that the pressure surface of the lower punch during a compression step has a normal shape, a cavity being defined between the die and the lower punch, said method comprising the steps of: moving one or more selected punch segments upward such a position that their pressure surface is positioned relatively higher than the pressure surface of the remaining punch segments, filling the cavity with the alloy powder, moving the selected punch segments downward until they join with the remaining punch segments to assume the normal shape of the lower punch during the compression step, compressing the alloy powder in the cavity between the upper and lower punches, while the normal shape of the pressure surface of the lower punch is maintained, under a magnetic field for uniaxial pressure molding to form a compact, and heat treating the compact, wherein in the step of moving the selected punch segments downward, the selected punch segments are moved down while a magnetic field is applied.
2. The method of claim 1, further comprising, after the pressure molding step, the step of withdrawing the compact from the die by relatively moving the upper and lower punches and the die while the compact in the mold is kept under pressure by both of the upper and lower punches.
3. The method of claim 2 wherein during the step of withdrawing the compact, the pressure on the compact is increased or decreased when the upper and lower punches and the die are relatively moved.
4. The method of claim 1 wherein the top of the alloy powder is leveled during or after the filling step.
5. The method of claim 1 wherein the selected punch segments are disposed at positions where the vertical thickness of the compact is thin.
6. The method of claim 1 wherein at least a portion of the pressure surface of one or both of the upper and lower punches is a curved surface of arch or inverse arch shape.
7. The method of claim 1 wherein the pressure surface of the upper punch is a curved surface of arcuate arch shape.
8. The method of claim 7 wherein the pressure surface of the lower punch consist of a central surface section having parallel side edges and two flanks extending from the side edges of the central surface section.
9. The method of claim 8 wherein the central surface section is a horizontal surface or a curved surface of arcuate arch shape, and the flank is a horizontal surface or a curved or flat surface inclined toward the convex side of the arch.
10. The method of claim 8 wherein the selected punch segments of the lower punch are two punch segments having a pressure surface corresponding to the flanks, and the remaining is one punch segment having a pressure surface corresponding to the central surface section.
11. The method of claim 2, further comprising, between the step of filling and the step of moving the selected punch segments downward, the steps of moving the die upward and/or the overall lower punch downward, and then resting the upper punch on top of the alloy powder.
12. The method of claim 1 wherein the lower punch is divided into two punch segments corresponding to said selected punch segments, and one punch segment corresponding to said remaining punch segment and providing the central section of the pressure surface of the lower punch.
13. The method of claim 12 wherein, in the step of withdrawing, the pressure applied to the compact, in each molding step and per compact, is 0.01 to 0.5 MPa/cm.sup.2 of a transverse section of the die perpendicular to the pressure application direction.
14. The method of claim 1 wherein the pressure surface of the upper punch is shaped non-planar.
15. The method of claim 14 being for preparing a rare earth sintered magnet having ID shape.
16. The method of claim 14 wherein the pressure surface of the lower punch is shaped non-planar.
17. The method of claim 16 being for preparing a rare earth sintered magnet having C shape.
18. The method of claim 14 wherein the upper punch has a downward pressure surface corresponding to the upper surface of the magnet, and the lower punch has an upward pressure surface corresponding to the lower surface of the magnet.
19. The method of claim 1 wherein, in the step of heat treating, the compact is sintered in a heat treatment furnace in high vacuum or a non-oxidizing gas atmosphere at a temperature of 1,000 to 1,200 C. for 1 to 10 hours.
Description
BRIEF DESCRIPTION OF DRAWINGS
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(7) In the following description, like reference characters designate like or corresponding parts throughout the several views shown in the figures. It is also understood that the terms upper, lower, upward, downward, and analogues are often used with reference to the vertical cross-sectional views of
DESCRIPTION OF PREFERRED EMBODIMENTS
(8) By the method of the invention, a rare earth sintered magnet is prepared by feeding a rare earth magnet-forming alloy powder into a mold cavity until the cavity is filled with the alloy powder, and compressing the alloy powder under a magnetic field. The method is best suited for the preparation of magnets having a non-planar shaped surface, typically curved surface, that is, of unique shape, typically C or D shape. The method for preparing a rare earth sintered magnet relies on compression molding using a mold comprising a die, an upper punch having a pressure surface, and a lower punch having a pressure surface. The pressure surface of one or both of the upper and lower punches is shaped non-planar, depending on the unique shape of a magnet to be prepared such as C or D shape.
(9) Specifically, when a sintered magnet 1 of C shape as shown in
(10) The non-planar shapes of upper and lower punches are not limited to the shapes of upper and lower punches 22 and 23 shown in
(11) The non-planar shape may also be such that a portion of the pressure surface is a curved surface of dome, inverse dome, arch or inverse arch shape while the remainder is a curved surface of different shape or a planar surface. Exemplary are a shape consisting of a curved surface segment of dome or inverse dome shape and an outer circumferential segment extending outward from the periphery of the curved surface segment, and a shape consisting of a curved surface segment of arch shape (e.g., arcuate arch shape) or inverse arch shape (e.g., arcuate inverse arch shape) and two flank segments extending outward from the opposite edges of the curved surface segment. The outer circumferential segment or flank segments may be either curved or planar. The extending outer circumferential segment or flank segments may be inclined toward the convex side of dome, inverse dome, arch or inverse arch shape, or inclined opposite to the convex side, or horizontal.
(12) According to the invention, the lower punch is divided into a plurality of punch segments which are independently movable within the die in the compression direction. Preferably 2 to 10, typically 2 or 3 divided punch segments are received in the die for single motion in a vertical direction. When it is desired to prepare a sintered magnet of C shape as shown in
(13) For use in the magnet preparation method of the invention, another mold as shown in
(14) In either of the molds of
(15) The invention may be applied to the preparation of either Nd-based or Sm-based rare earth sintered magnets. When the invention is applied to Nd-based rare earth sintered magnets, exemplary is an alloy composition consisting of 20 to 35% by weight of R which is at least one rare earth element selected from Nd, Pr, Dy, Tb and Ho, up to 15% by weight of Co, 0.2 to 8% by weight of B, up to 8% by weight of at least one additive element selected from Ni, Nb, Al, Ti, Zr, Cr, V, Mn, Mo, Si, Sn, Ga, Cu and Zn, and the balance of Fe, and incidental impurities. A rare earth sintered magnet-forming alloy powder preferably has an average particle size of 1 to 10 m after fine milling on a jet mill or the like. The average particle size may be determined, for example, by the laser light diffraction method as a median diameter.
(16) The invention uses the mold including the die, the upper punch, and the lower punch composed of a plurality of divided punch segments. A cavity is defined between the die and the lower punch. The mold cavity is filled with the alloy powder when selected punch segments (first punch segments) are moved up such that their pressure surface is positioned relatively higher than the pressure surface of the remaining punch segments (second punch segment). Where the mold shown in
(17) Although the step of filling the cavity with the alloy powder is not particularly limited, the cavity is typically filled with the alloy powder 11 up to a level corresponding to the upper edge of the die 21 as shown in
(18) Once the cavity is filled with the alloy powder, the selected punch segments (first punch segments) are moved down until the selected punch segments (first punch segments) join with the remaining punch segments (second punch segment) to assume the normal shape of the lower punch during the compression step. Where the mold shown in
(19) With this downward movement of selected punch segments (first punch segments), the alloy powder on the selected punch segments (first punch segments) is also moved down. The procedure of once moving upward selected punch segments (first punch segments), filling the cavity with the alloy powder, and then moving downward the selected punch segments (first punch segments) ensures that the amount of the alloy powder deposited at the position where the vertical thickness of the compact (and hence, magnet) is thin is reduced (that is, the height of the alloy powder is reduced). As a result, the density of the compact (and hence, magnet) is made uniform throughout, which is effective for preventing the compact from warp, deformation, cracks, and fissures. In this sense, it is advantageous to locate selected punch segments (first punch segments) at the position where the vertical thickness of the compact is thin.
(20) After the selected punch segments (first punch segments) are moved downward (
(21) In the practice of the invention, the step of moving downward the selected punch segments (first punch segments) is preferably carried out while a magnetic field is applied across the alloy powder. In the preferred procedure, the upper punch 22 is rested on top of the alloy powder 11 as shown in
(22) Since the selected punch segments (first punch segments) are moved downward under the applied magnetic field, alloy powder particles deposited on the selected punch segments (first punch segments) descend while the particles are kept magnetized, dispersed and oriented. If the packing density of alloy powder particles deposited on the selected punch segments (first punch segments) is equal to the packing density of alloy powder particles deposited on the remaining punch segments (second punch segment), those alloy powder particles on the selected punch segments descend with the packing density maintained. If the packing density of alloy powder particles deposited on the remaining punch segments (second punch segment) is higher than the packing density of alloy powder particles deposited on the selected punch segments (first punch segments), some powder particles shift from the remaining punch segment (second punch segment) side to the selected punch segment (first punch segment) side as alloy powder particles descend, achieving uniformity of packing density. A uniform packing density is available in either case.
(23) After the selected punch segments (first punch segments) are moved down (
(24) After the compression molding step mentioned above, the compact is removed from the mold. Preferably the compact is withdrawn from the die by relatively moving the upper and lower punches and the die while the compact in the mold is kept compressed by the upper and/or lower punch. For example, the compact 1a resulting from uniaxial compression molding in a magnetic field as shown in
(25) The step of withdrawing the compact from the die while keeping the compact under pressure ensures to prevent the compact from cracking and fissure. The pressure applied to the compact, in each molding step and per compact, is preferably up to 0.5 MPa/cm.sup.2, more preferably up to 0.2 MPa/cm.sup.2, and even more preferably up to 0.15 MPa/cm.sup.2, and at least 0.01 MPa/cm.sup.2, more preferably at least 0.05 MPa/cm.sup.2 of a transverse section of the die perpendicular to the pressure application direction. The pressure applied during the withdrawing step is preferably equal to or lower than the pressure applied during the compression molding step. Once the pressure applied during the compression molding step is released (i.e., to zero), the pressure necessary for the withdrawing step may be set by applying a predetermined pressure again. However, the pressure necessary for the withdrawing step is preferably set by releasing the pressure applied during the compression molding step in a controlled manner until the predetermined pressure is reached. The pressure applied to the compact may be kept constant during the relative movement of the upper and lower punches and the die, or increased or decreased midway the relative movement.
(26) In the step of compression molding the alloy powder in the mold cavity, a magnetic field of 1.0 to 2.5 T may be applied. The pressure applied to the fill, in each molding step and per compact, may be at least 0.1 MPa/cm.sup.2, more preferably at least 0.15 MPa/cm.sup.2 and up to 1 MPa/cm.sup.2, more preferably up to 0.9 MPa/cm.sup.2 of a transverse section of the die perpendicular to the pressure application direction.
(27) Finally, the compact is heat treated into a sintered rare earth magnet. Specifically, the compact is sintered in a heat treatment furnace in high vacuum or a non-oxidizing gas atmosphere such as argon at a temperature of 1,000 to 1,200 C. for 1 to 10 hours. The sintering may be followed by further heat treatment (aging treatment) in vacuum or a non-oxidizing gas atmosphere such as argon at a lower temperature than the sintering temperature, preferably 400 to 700 C.
EXAMPLE
(28) Examples are given below for further illustrating the invention although the invention is not limited thereto.
Example 1
(29) A neodymium-based magnet alloy consisting of 25.0 wt % Nd, 7.0 wt % Pr, 1.0 wt % Co, 1.0 wt % B, 0.2 wt % Al, 0.1 wt % Zr, 0.2 wt % Cu, and the balance of Fe was coarsely crushed by hydrogen decrepitation and finely milled on a jet mill, obtaining a fine powder having an average particle size of 3.0 m. Sintered rare earth magnets were prepared from this alloy powder, using a molding apparatus including a mold configured as shown in
(30) First the die 21 was combined with the lower punch 23 to define a cavity. Two first punch segments 23a, 23b were moved up and positioned such that the pressure surface of the first punch segments 23a, 23b was 17 mm higher than the pressure surface of the second punch segment 23c, rather than the normal shape that the pressure surface of the lower punch 23 should take during the compression step. Next, the mold cavity was filled with the alloy powder up to the upper edge of the die 21 so that the alloy powder 11 had a height of 40 mm. The top of the alloy powder was leveled.
(31) Next, the die 21 was slightly moved up until a space was created above the alloy powder 11. The upper punch 22 was inserted in the die space and rested on the alloy powder 11. The first punch segments 23a, 23b were moved down 17 mm. At this position, the first punch segments 23a, 23b and the second punch segment 23c together assumed the normal shape of the lower punch 23 during the subsequent compression step.
(32) Next, the alloy powder was compression molded in a magnetic field of 1.5 T and under a pressure of 0.3 MPa/cm.sup.2 into a compact. The pressure was gradually released to a certain level. While the compact was kept under a pressure of 0.05 MPa/cm.sup.2, 0.1 MPa/cm.sup.2, or 0.15 MPa/cm.sup.2 between the upper and lower punches 22 and 23, the die 21 was moved down until the compact was withdrawn from the die 21. The compact of C shape as shown in
(33) The compacts were placed in a heat treatment furnace where they were sintered in vacuum at 1,040 C. for 3 hours, followed by heat treatment in vacuum at 480 C. for 3 hours. In this way, there were obtained 30 sintered magnets. After surface polishing, the magnets were inspected for cracks in the interior (bulk cracks) and cracks on the surface (surface cracks). The number of bulk cracked magnet samples and surface cracked magnet samples was counted, with the results shown in Table 1.
Example 2
(34) Sintered rare earth magnets were prepared as in Example 1 except that the pressure surface of the first punch segments 23a, 23b was set 20 mm higher than the pressure surface of the second punch segment 23c prior to the filling step, and the alloy powder had a height of 41.5 mm. The number of cracked samples was similarly counted, with the results shown in Table 1.
Comparative Example 1
(35) Sintered rare earth magnets were prepared as in Example 1 except that the first punch segments 23a, 23b were not moved up prior to the filling step, and the alloy powder had a height of 33 mm. The number of cracked samples was similarly counted, with the results shown in Table 1.
Comparative Example 2
(36) Sintered rare earth magnets were prepared as in Example 1 except that the first punch segments 23a, 23b were not moved up prior to the filling step, and the alloy powder had a height of 40 mm. The number of cracked samples was similarly counted, with the results shown in Table 1.
(37) TABLE-US-00001 TABLE 1 Pressure Moved up Fill during Bulk Surface height height withdrawal cracked cracked (mm) (mm) (MPa/cm.sup.2) samples samples Example 1 17 40 0.05 7/30 0/30 0.1 0/30 0/30 0.15 0/30 3/30 Example 2 20 41.5 0.05 3/30 0/30 0.1 0/30 0/30 0.15 0/30 2/30 Comparative 0 33 0.05 9/30 0/30 Example 1 0.1 0/30 7/30 0.15 0/30 10/30 Comparative 0 40 0.05 12/30 0/30 Example 2 0.1 2/30 6/30 0.15 0/30 15/30
(38) It is evident that the magnets prepared in Examples 1 and 2 are improved in crack control over the magnets prepared in Comparative Examples 1 and 2.
Comparative Example 3
(39) Sintered rare earth magnets were prepared as in Example 1 except that after compression molding, the pressure was fully released to 0 MPa, and the compact was withdrawn from the die without applying any pressure to the compact by the upper and lower punches. The number of cracked samples was similarly counted, with the results shown in Table 2.
Comparative Example 4
(40) Sintered rare earth magnets were prepared as in Example 2 except that after compression molding, the pressure was fully released to 0 MPa, and the compact was withdrawn from the die without applying any pressure to the compact by the upper and lower punches. The number of cracked samples was similarly counted, with the results shown in Table 2.
(41) TABLE-US-00002 TABLE 2 Pressure Moved up Fill during Bulk Surface height height withdrawal cracked cracked (mm) (mm) (MPa/cm.sup.2) samples samples Comparative 17 40 0 30/30 0/30 Example 3 Comparative 20 41.5 0 30/30 0/30 Example 4
(42) The magnets prepared in Comparative Examples 3 and 4 without applying any pressure to the compact upon withdrawal from the die showed a bulk cracked sample count of 100%. For the magnets prepared in Examples 1 and 2 wherein the compact was withdrawn from the die while keeping the compact under a certain pressure, bulk cracking was controlled.
Example 3
(43) Sintered rare earth magnets were prepared as in Example 1 except that a magnetic field of 1.5 T was applied when the first punch segments 23a, 23b were moved down to the position where the first punch segments 23a, 23b and the second punch segment 23c together assumed the normal shape of the lower punch 23 during the compression step. The number of cracked samples was similarly counted, with the results shown in Table 3.
(44) TABLE-US-00003 TABLE 3 Pressure Moved up Fill during Bulk Surface height height withdrawal cracked cracked (mm) (mm) (MPa/cm.sup.2) samples samples Example 3 17 40 0.05 0/30 0/30 0.1 0/30 0/30 0.15 0/30 2/30
(45) As is evident from the results of Example 3, crack formation is further controlled by moving down the first punch segments in an applied magnetic field.
(46) Japanese Patent Application No. 2014-080219 is incorporated herein by reference.
(47) Although some preferred embodiments have been described, many modifications and variations may be made thereto in light of the above teachings. It is therefore to be understood that the invention may be practiced otherwise than as specifically described without departing from the scope of the appended claims.