R-T-B based alloy strip, and R-T-B based sintered magnet and method for producing same

Abstract

An R-T-B based alloy strip including columnar crystals of an R.sub.2T.sub.14B phase, wherein in a cross-section along the thickness direction, columnar crystals extend out in a radial fashion from the crystal nuclei, the R-T-B based alloy strip satisfying the following inequality (1), where D.sub.1 and D.sub.2 are, respectively, the average value for the lengths of the columnar crystals on one side and the average value for the lengths on the other side that is opposite the one side, in the direction perpendicular to the thickness direction of the cross-section.
0.9/1.1D.sub.2/D.sub.11.1/0.9(1)

Claims

1. An R-T-B based alloy strip comprising columnar crystals of an R.sub.2T.sub.14B phase, wherein R represents at least one element selected from the group consisting of rare earth elements, T represents at least one of iron and cobalt, and B represents boron, wherein in a cross-section along the thickness direction, columnar crystals extend out in a radial fashion from the crystal nuclei, the R-T-B based alloy strip satisfying the following inequality (1), where D.sub.1 and D.sub.2 are, respectively, the average value for the lengths of the columnar crystals on one side and the average value for the lengths on the other side that is opposite the one side, in the direction perpendicular to the thickness direction of the cross-section,
1D.sub.2/D.sub.11.1(1).

2. The R-T-B based alloy strip according to claim 1, satisfying the following inequalities (2) and (3), where D.sub.AVE and D.sub.MAX are, respectively, the average value and the maximum value for the lengths of the columnar crystals in the direction perpendicular to the thickness direction in the cross-section
1.0 mD.sub.AVE3.0 m(2)
1.5 mD.sub.MAX4.5 m(3).

3. The R-T-B based alloy strip according to claim 1, containing an R-rich phase in which the R content is higher than the R.sub.2T.sub.14B phase based on mass, the percentage of the number of R-rich phases with lengths of no greater than 1.5 m in the direction perpendicular to the thickness direction, with respect to the total number of R-rich phases, in the cross-section, being 90% or greater.

4. An R-T-B based sintered magnet obtained by molding and firing alloy powder obtained by grinding the R-T-B based alloy strip according to claim 1.

5. A method for producing an R-T-B based sintered magnet, the method comprising the steps of: grinding the R-T-B based alloy strip according to claim 1 to prepare an alloy powder, and molding and firing the alloy powder to produce the R-T-B based sintered magnet.

6. A method for producing an R-T-B based sintered magnet, the method comprising the steps of: grinding the R-T-B based alloy strip according to claim 2 to prepare an alloy powder, and molding and firing the alloy powder to produce the R-T-B based sintered magnet.

Description

BRIEF DESCRIPTION OF DRAWINGS

(1) FIG. 1 is a schematic cross-sectional enlarged view of a section of a cross-section of an R-T-B based alloy strip according to an embodiment of the invention, along the thickness direction.

(2) FIG. 2 is a schematic diagram showing an example of a method for producing an alloy strip according to the invention.

(3) FIG. 3 is an enlarged plan view showing an example of the roll surface of a cooling roll used for production of an alloy strip according to the invention.

(4) FIG. 4 is a schematic cross-sectional view showing an example of the cross-sectional structure near the roll surface of a cooling roll used for production of an alloy strip according to the invention.

(5) FIG. 5 is a schematic cross-sectional view showing an example of the cross-sectional structure near the roll surface of a cooling roll used for production of an alloy strip according to the invention.

(6) FIG. 6 is a SEM-BEI photograph (magnification: 350) of a cross-section of an alloy strip according to an embodiment of the invention, along the thickness direction.

(7) FIG. 7 is a cross-sectional view schematically showing an example of the cross-sectional structure of an R-T-B based sintered magnet according to an embodiment of the invention.

(8) FIG. 8 is an illustration showing the internal structure of a motor comprising an R-T-B based sintered magnet according to an embodiment of the invention.

(9) FIG. 9 is an SEM-BEI photograph (magnification: 350) of a cross-section of the R-T-B based alloy strip of Example 5, along the thickness direction.

(10) FIG. 10 is an SEM-BEI photograph (magnification: 350) of a cross-section of the R-T-B based alloy strip of Comparative Example 3, along the thickness direction.

(11) FIG. 11 is a schematic cross-sectional enlarged view showing the cross-sectional structure of a conventional R-T-B based alloy strip along the thickness direction.

(12) FIG. 12 is a diagram showing element map data for the rare earth sintered magnet of Example 10, with the triple point regions indicated in black.

(13) FIG. 13 is a diagram showing element map data for the R-T-B based sintered magnet of Comparative Example 4, with the triple point regions indicated in black.

DESCRIPTION OF EMBODIMENTS

(14) Preferred embodiments of the invention will now be explained with reference to the accompanying drawings where necessary. For the drawings, identical or corresponding elements will be referred to by like reference numerals and will be explained only once.

(15) <R-T-B Based Alloy Strip>

(16) FIG. 1 is a schematic cross-sectional enlarged view showing the cross-sectional structure of an R-T-B based alloy strip of this embodiment along the thickness direction. The R-T-B based alloy strip of this embodiment contains R.sub.2T.sub.14B phase columnar crystals 2 as the main phase and a grain boundary phase 4 having a different structure than the R.sub.2T.sub.14B phase. The grain boundary phase 4 includes, for example, an R-rich phase. An R-rich phase is a phase with a higher R content than the R.sub.2T.sub.14B phase.

(17) As shown in FIG. 1, the R-T-B based alloy strip has crystal nuclei 1 on one surface. Also, the crystal nuclei 1 serve as origins from which the columnar crystals and grain boundary phase extend in a radial fashion toward the other surface. The grain boundary phase 4 is deposited along the grain boundaries of the R.sub.2T.sub.14B phase columnar crystals 2. Throughout the present specification, R represents elements including at least one selected from among rare earth elements, T represents elements including at least one of iron and cobalt, and B represents boron.

(18) The term rare earth element, for the purpose of the present specification, refers to scandium (Sc), yttrium (Y) and lanthanoid elements belonging to Group 3 of the long Periodic Table, the lanthanoid elements including, for example, lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb) and lutetium (Lu).

(19) The R-T-B based alloy strip of this embodiment does not have significant spread of the R.sub.2T.sub.14B phase columnar crystals 2 in the direction perpendicular to the thickness direction (the left-right direction in FIG. 1), in a cross-section along the thickness direction as shown in FIG. 1, but instead they grow essentially uniformly in the thickness direction (the up-down direction in FIG. 1). Consequently, the widths of R.sub.2T.sub.14B phase columnar crystals 2, i.e. the lengths M in the left-right direction, are smaller compared to a conventional R-T-B based alloy strip as shown in FIG. 11, and variation in the lengths M is reduced. The widths of the R-rich phase 4, i.e. the lengths in the left-right direction are also small, and variation in the lengths is reduced.

(20) The R-T-B based alloy strip of this embodiment satisfies the following inequality (1), where D.sub.1 and D.sub.2 are, respectively, the average value for the lengths of the columnar crystals 2 on one (lower) surface side, in the direction perpendicular to the thickness direction of the R-T-B based alloy strip, i.e. the left-right direction in FIG. 1, and the average value for the lengths of the columnar crystals 2 on the other (upper) surface side, in the cross-section shown in FIG. 1.
0.9/1.1D.sub.2/D.sub.11.1/0.9(1)

(21) Throughout the present specification, D.sub.1, D.sub.2 and D.sub.3 are determined as follows. D.sub.3 is the average value for the lengths of the center sections of the columnar crystals 2 in the direction perpendicular to the thickness direction of the R-T-B based alloy strip, in a cross-section as shown in FIG. 1.

(22) First, a cross-section such as shown in FIG. 1 is observed by SEM (scanning electron microscope)-BEI (backscattered electron image) (magnification: 1000). Photographs are taken of the cross-section in 15 visual fields, on one surface side of the R-T-B based alloy strip, on the other surface side which is the surface opposite the one surface, and on the center section. In the photographs, straight lines are drawn between a location 50 m on the center section side from the one surface, a location 50 m on the center section side from the other surface, and the center section. The straight lines are essentially parallel to the one surface and the other surface in the cross-section shown in FIG. 1. The values of D.sub.1, D.sub.2 and D.sub.3 can be determined from the lengths of the straight lines and the number of columnar crystals 2 transected by the straight lines.

(23) Since D.sub.2/D.sub.1 for the R-T-B based alloy strip of this embodiment satisfies formula (1) above, the widths and shapes of the columnar crystals 2 have low variation and high homogeneity in the thickness direction. From the viewpoint of further increasing the homogeneity, the value of D.sub.2/D.sub.1 preferably satisfies the following inequality (4) and more preferably satisfies the following inequality (5).
0.95/1.05D.sub.2/D.sub.11.05/0.95(4)
0.98/1.02D.sub.2/D.sub.11.02/0.98(5)

(24) The R-T-B based alloy strip of this embodiment may be produced by a strip casting method using a cooling roll as described below. In this case, R.sub.2T.sub.14B phase crystal nuclei 1 of the R-T-B based alloy strip are deposited on the contact surface with the cooling roll (the casting surface). The R.sub.2T.sub.14B phase columnar crystals 2 grow in a radial fashion from the casting surface side of the R-T-B based alloy strip toward the side opposite the casting surface (the free surface). Thus, in the R-T-B based alloy strip shown in FIG. 1, the lower surface is the casting surface. In this case, D.sub.1 is the average value for the lengths of the columnar crystals 2 on the casting surface side, and D.sub.2 is the average value for the lengths of the columnar crystals 2 on the free surface side. In most cases, the relationship D.sub.2D.sub.1 applies.

(25) When the relationship D.sub.2D.sub.1 applies for the R-T-B based alloy strip of this embodiment, the values of D.sub.1 and D.sub.2 preferably satisfy inequality (6) below. This allows the widths of the R.sub.2T.sub.14B phase columnar crystals 2, i.e. the lengths M in the left-right direction, to be sufficiently small, and variation in the lengths M to be sufficiently reduced. It also allows an R-T-B based sintered magnet to be obtained having minimized segregation of the R-rich phase as well as increased homogeneity of the microstructure.
1D.sub.2/D.sub.11.1(6)

(26) When D.sub.2D.sub.1, the lower limit for D.sub.2/D.sub.1 is preferably 1.01 and more preferably 1.02. The upper limit for D.sub.2/D.sub.1 is preferably 1.09 and more preferably 1.05.

(27) The values of D.sub.1, D.sub.2 and D.sub.3 are, for example, 1 to 4 m, preferably 1.4 to 3.5 m, and more preferably 1.5 to 3.2 m. If the values of D.sub.1, D.sub.2 and D.sub.3 are large, it will tend to be difficult to sufficiently micronize the alloy powder that is obtained by grinding. On the other hand, an R-T-B based alloy strip with excessively low values for D.sub.1, D.sub.2 and D.sub.3, while maintaining columnar crystal shapes, will generally be difficult to produce.

(28) The R-T-B based alloy strip of this embodiment preferably satisfies the following inequalities (2) and/or (3), where D.sub.AVE and D.sub.MAX are, respectively, the average value and maximum value for the lengths of the columnar crystals 2 in the direction perpendicular to the thickness direction, in the cross-section shown in FIG. 1.
1.0 mD.sub.AVE3.5 m(2)
1.5 mD.sub.MAX4.5 m(3)

(29) Throughout the present specification, D.sub.AVE is the average value for D.sub.1, D.sub.2 and D.sub.3 determined from the results of the aforementioned SEM-BEI image observation (magnification: 1000). Thus, D.sub.AVE is the average value for the lengths of the columnar crystals 2 along the direction perpendicular to the thickness direction, over the entire cross-section shown in FIG. 1. Throughout the present specification, D.sub.MAX is the length of columnar crystals 2 in the photograph where the lengths of the columnar crystals 2 are at a maximum, among a total of 45 photographs taken for each of 15 visual fields, on the one surface side, the other surface side and the center section.

(30) Specifically, inequality (2) specifies that the sizes (widths) of the columnar crystals 2 are in a prescribed range, and inequality (3) specifies that the variation in the sizes (widths) of the columnar crystals 2 is within a prescribed range. An R-T-B based alloy strip satisfying inequalities (2) and (3) is composed of columnar crystals 2 that are further micronized and have sufficiently reduced variation in shapes and sizes, and an R-rich phase 4 that is further micronized and has sufficiently reduced variation in shapes and sizes. Consequently, using alloy powder obtained by grinding such an R-T-B based alloy strip can yield an R-T-B based sintered magnet with further inhibited segregation of the R-rich phase and further increased microstructural homogeneity. If D.sub.AVE and D.sub.MAX are too small, ultrafine powder will increase during fine grinding, and the amount of oxygen will tend to increase. Also, chill crystals, which are equiaxial crystals, will also increase, and when a sintered magnet is formed the residual flux density (Br) will tend to be lowered.

(31) From the viewpoint of obtaining an R-T-B based sintered magnet that is even more micronized and has a uniform structure, D.sub.AVE and D.sub.MAX preferably satisfy the following inequalities (7) and (8). The R-T-B based alloy strip will thus be one that can yield an R-T-B based sintered magnet having an even more micronized structure, while also facilitating production of the R-T-B based alloy strip.
1.0 mD.sub.AVE2.4 m(7)
1.5 mD.sub.MAX3.0 m(8)

(32) From the viewpoint of obtaining an R-T-B based sintered magnet that has an even more micronized structure and facilitating production of the R-T-B based alloy strip, D.sub.AVE and D.sub.MAX preferably satisfy the following inequalities (9) and (10).
1.5 mD.sub.AVE2.4 m(9)
2.0 mD.sub.MAX3.0 m(10)

(33) In the cross-section shown in FIG. 1, the proportion of the number of R-rich phases 4 with lengths of no greater than 1.5 m in the direction perpendicular to the thickness direction, with respect to all of the R-rich phases 4, as phases with a high rare earth element concentration, is preferably 90% or greater, more preferably 93% or greater and even more preferably 95% or greater. By thus increasing the proportion of the number of R-rich phases 4 with lengths of no greater than 1.5 m in the columnar crystals 2 in the R-T-B based alloy strip, it is possible to obtain an R-T-B based sintered magnet with even higher coercive force.

(34) <Method for Producing R-T-B Based Alloy Strip>

(35) FIG. 2 is a schematic diagram of an apparatus for production of the R-T-B based alloy strip of this embodiment. The R-T-B based alloy strip of this embodiment may be produced by a strip casting method using a production apparatus such as shown in FIG. 2. The method for producing an alloy strip according to this embodiment comprises a melting step in which a molten R-T-B based alloy is prepared, a first cooling step in which the molten alloy is poured onto the roll surface of the cooling roll rotating in the circumferential direction, cooling the molten alloy by the roll surface to produce crystal nuclei, and solidifying at least a portion of the molten alloy, and a second cooling step in which the alloy containing crystal nuclei is further cooled to obtain an alloy strip. Each of these steps will now be explained in detail.

(36) In the melting step, a starting material comprising at least one rare earth metal or rare earth alloy, or pure iron, ferroboron or an alloy thereof, is introduced into a high-frequency melting furnace 10. In the high-frequency melting furnace 10, the starting material is heated to 1300 C. to 1500 C. to prepare a molten alloy 12.

(37) In the first cooling step, the molten alloy 12 is transferred to a tundish 14. Next, the molten alloy is poured from the tundish 14 onto the roll surface of the cooling roll 56 rotating at a prescribed speed in the direction of the arrow A. The molten alloy 12 contacts with the roll surface 17 of the cooling roll 16 and loses heat by heat exchange. As the molten alloy 12 cools, crystal nuclei are formed in the molten alloy and at least part of the molten alloy 12 solidifies. For example, a R.sub.2T.sub.14B phase (melting temperature of about 1100 C.) is formed first, and then at least part of the R-rich phase (melting temperature of about 700 C.) solidifies. The crystal deposition is affected by the structure of the roll surface 17 with which the molten alloy 12 contacts. A concavoconvex pattern, comprising mesh-like recesses and raised sections formed by recesses, is formed on the roll surface 17 of the cooling roll 16.

(38) FIG. 3 is a schematic diagram showing a flat enlarged view of part of a roll surface 17. Mesh-like grooves are formed in the roll surface 17, and these form the concavoconvex pattern. Specifically, the roll surface 17 has a plurality of first recesses 32 arranged at a prescribed spacing a along the circumferential direction of the cooling roll 16 (the direction of the arrow A); and has a plurality of second recesses 34 arranged essentially perpendicular to the first recesses 32 and at a prescribed spacing b parallel to the axial direction of the cooling roll 16. The first recesses 32 and the second recesses 34 are essentially straight linear grooves having prescribed depths. Raised sections 36 are formed by the first recesses 32 and the second recesses 34.

(39) The angle formed by the first recesses 32 and second recesses 34 is preferably 80-100 and more preferably 85-95. By specifying such an angle , it will be possible for greater columnar growth of the crystal nuclei of the R.sub.2T.sub.14B phase deposited on the raised sections 36 of the roll surface 17 to proceed toward the thickness direction of the alloy strip.

(40) FIG. 4 is a schematic enlarged cross-sectional view showing a cross-section of FIG. 3 along line Iv-Iv. Specifically, FIG. 4 is a schematic cross-sectional view showing a portion of the cross-sectional structure of a cooling roll 16 cut through the axis on a plane parallel to the axial direction. The heights h1 of the raised sections 36 can be calculated as the shortest distances between the apexes of the raised sections 36 and a straight line L1 passing through the bases of the first recesses 32 and parallel to the axial direction of the cooling roll 16, in the cross-section shown in FIG. 5. Also, the spacing w1 of the raised sections 36 can be calculated as the distance between apexes of adjacent raised sections 36, in the cross-section shown in FIG. 4.

(41) FIG. 5 is a schematic enlarged cross-sectional view showing a cross-section of FIG. 3 along line V-V. Specifically, FIG. 5 is a schematic cross-sectional view showing a portion of the cross-sectional structure of a cooling roll 16 cut on a plane parallel to the side. The heights h2 of the raised sections 36 can be calculated as the shortest distances between the apexes of the raised sections 36 and a straight line L2 passing through the bases of the second recesses 34 and perpendicular to the axial direction of the cooling roll 16, in the cross-section shown in FIG. 5. Also, the spacing w2 of the raised sections 36 can be calculated as the distance between apexes of adjacent raised sections 36, in the cross-section shown in FIG. 5.

(42) Throughout the present specification, the average value H of the heights of the raised sections 36 and the average value W of the spacing between raised sections 36 are calculated in the following manner. Using a laser microscope, a profile image (magnification: 200) was taken of a cross-section of the cooling roll 16 near the roll surface 17, as shown in FIGS. 4 and 5. In these images, 100 points were measured for both heights h1 and heights h2 of arbitrarily selected raised sections 36. Here, measurement was made only for heights h1 and h2 that were 3 m or greater, including no data for heights of less than 3 m. The arithmetic mean value of measurement data for a total of 200 points was recorded as the average value for the heights of the raised sections 36.

(43) Also, in the same image, 100 points were measured for both spacings w1 and spacings w2 of arbitrarily selected raised sections 36. Measurement of the spacings was conducted considering only heights h1 and h2 of 3 m and greater as raised sections 36. The arithmetic mean value of measurement data for a total of 200 points was recorded as the average value W for the spacings of the raised sections 36. When it is difficult to observe a concavoconvex pattern on the roll surface 17 with a scanning electron microscope, a replica may be formed by replicating the concavoconvex pattern of the roll surface 17, and the surface of the replica observed with a scanning electron microscope and measured as described above. A replica can be formed using a commercially available kit (SUMP SET by Kenis, Ltd.).

(44) The concavoconvex pattern of the roll surface 17 can be adjusted by working the roll surface 17 with a short wavelength laser, for example.

(45) The average value H of the heights of the raised sections 36 is preferably 7 to 20 m. This will cause the recesses 32, 34 to be thoroughly saturated with the molten alloy and allow adhesiveness between the molten alloy 12 and roll surface 17 to be sufficiently increased. The upper limit for the average value H is more preferably 16 m and even more preferably 14 m, from the viewpoint of more thoroughly saturating the recesses 32, 34 with the molten alloy. The lower limit for the average value H is more preferably 8.5 m and even more preferably 8.7 m, from the viewpoint of obtaining R.sub.2T.sub.14B phase crystals with sufficiently high adhesiveness between the molten alloy and the roll surface 17, while also having more uniform orientation in the thickness direction of the alloy strip.

(46) The average value W of the spacing between raised sections 36 is 40 to 100 m. The upper limit for the average value W is preferably 80 m, more preferably 70 m and even more preferably 67 m, from the viewpoint of further reducing the widths of the R.sub.2T.sub.14B phase columnar crystals and obtaining magnet powder with a small particle diameter. The lower limit for the average value W is preferably 45 m and more preferably 48 m. This will allow an R-T-B based sintered magnet to be obtained having even higher magnetic properties.

(47) The surface roughness Rz of the roll surface 17 is preferably 3 to 5 m, more preferably 3.5 to 5 m and even more preferably 3.9 to 4.5 m. If Rz is too large the thickness of the strip will vary tending to increase variation in the cooling rate, whereas if Rz is too small, adhesiveness between the molten alloy and the roll surface 17 will be insufficient, and the molten alloy or alloy strip will tend to detach from the roll surface 17 earlier than the target time. In this case, the molten alloy migrates to the secondary cooling section 20 without sufficient progression of heat loss of the molten alloy. Therefore, the alloy strips 18 will sometimes stick together at the secondary cooling section 20.

(48) The surface roughness Rz, for the purpose of the present specification, is the ten-point height of irregularities and is the value measured according to JIS B 0601-1994. Rz can be measured using a commercially available measuring apparatus (SURFTEST by Mitsutoyo Corp.).

(49) For this embodiment, a cooling roll 16 having a roll surface 17 such as shown in FIGS. 3 to 5 is used, and therefore when the molten alloy 12 is poured onto the roll surface 17 of the cooling roll 16, the molten alloy 12 first contacts with the raised sections 36. Crystal nuclei 1 are generated at the contact sections, and the crystal nuclei 1 serve as origins for growth of R.sub.2T.sub.14B phase columnar crystals 2. By increasing the number of crystal nuclei 1 per unit area by generation of numerous such crystal nuclei 1, it is possible to minimize growth of the columnar crystals 2 along the roll surface 17.

(50) The cooling roll 16 and roll surface 17 have prescribed heights and have raised sections 36 arranged in a prescribed spacing. Numerous R.sub.2T.sub.14B phase crystal nuclei 1 are generated on the roll surface 17, after which the columnar crystals 2 grow in a radial fashion with the crystal nuclei 1 as origins. During this time, growth of the columnar crystals 2 proceeds in the thickness direction of the R-T-B based alloy strip, forming R.sub.2T.sub.14B phase columnar crystals 2 with small widths and low variation in width and shape, and R-rich phases 4 that are even more micronized and have sufficiently reduced variation in shape and size.

(51) The cooling rate in the first cooling step is preferably 1000 C. to 3000 C./sec and more preferably 1500 C. to 2500 C./sec, from the viewpoint of adequately micronizing the structure of the obtained alloy strip while inhibiting generation of heterophases. If the cooling rate is below 1000 C./sec, an a-Fe phase will tend to be readily deposited, and if the cooling rate exceeds 3000 C./sec, chill crystals will tend to be readily deposited. Chill crystals are isotropic microcrystals with particle diameters of 1 m and smaller. High generation of chill crystals tends to impair the magnetic properties of the finally obtained R-T-B based sintered magnet.

(52) The cooling rate can be controlled, for example, by adjusting the temperature or flow rate of cooling water flowing through the interior of the cooling roll 16. The cooling rate can also be adjusted by varying the material of the roll surface 17 of the cooling roll 16. The material used for the cooling roll may be a copper sheet with a purity of 95 mass %, for example.

(53) The second cooling step is a step in which the alloy strip 18 containing the crystal nuclei generated by the first cooling step is further cooled by a secondary cooling section 20. There are no particular restrictions on the cooling method in the second cooling step, and any conventional cooling method may be employed. For example, the secondary cooling section 20 may be one provided with a gas tube 19 having a gas blow hole 19a, wherein cooling gas is blown through the gas blow hole 19a onto the alloy strip accumulated on a rotating table rotating in the circumferential direction. The alloy strip 18 can be sufficiently cooled in this manner. The alloy strip is recovered after sufficient cooling with the secondary cooling section 20.

(54) The thickness of the R-T-B based alloy strip of this embodiment is preferably no greater than 0.5 mm and more preferably 0.1 to 0.5 mm. If the thickness of the alloy strip becomes too large, the difference in cooling rate will tend to roughen the columnar crystal structure and impair the homogeneity. Also, the structure near the surface on the roll surface 17 side (the casting surface) and the structure near the surface on the side opposite the casting surface (the free surface) of the alloy strip will differ, and the difference between D.sub.1 and D.sub.2 will tend to increase.

(55) The R-T-B based alloy strip of this embodiment comprises an R.sub.2T.sub.14B phase as the main phase and an R-rich phase as the heterophase. Here, the main phase is the crystal phase most abundantly present in the alloy strip, while the heterophase is the crystal phase different from the main phase and is the crystal phase primarily present at the grain boundaries of the main phase. The R-rich phase is a phase that is non-magnetic and has a higher R content based on mass than the R.sub.2T.sub.14B phase. The R-T-B based alloy strip of this embodiment may also contain an a-Fe phase and chill crystals in addition to the R-rich phase as the heterophase. However, the total heterophase content is preferably no greater than 10 mass %, more preferably no greater than 7 mass % and even more preferably no greater than 5 mass %, with respect to the total R-T-B based alloy strip. By thus reducing the total heterophase content, it is possible to obtain an R-T-B based sintered magnet with both excellent residual flux density and coercive force.

(56) FIG. 6 is a SEM-BEI image photograph showing a cross-section of an R-T-B based alloy strip in the thickness direction. FIG. 6(A) is an SEM-BEI image photograph (magnification: 350) showing a cross-section of the R-T-B based alloy strip of this embodiment in the thickness direction. Also, FIG. 6(B) is an SEM-BEI image photograph (magnification: 350) showing a cross-section of a conventional R-T-B based alloy strip in the thickness direction. In FIGS. 6(A) and (B), the lower side surface of the R-T-B based alloy strip is the contact surface with the roll surface 17 (casting surface). Also, in FIGS. 6(A) and (B) the black sections represent R.sub.2T.sub.14B phases and the white sections represent R-rich phases.

(57) As shown in FIG. 6(A), the R-T-B based alloy strip of this embodiment has the crystal nuclei of numerous R.sub.2T.sub.14B phases deposited on the lower surface (see the arrows in the drawing). In addition, R.sub.2T.sub.14B phase columnar crystals extend in a radial fashion from the crystal nuclei in the upward direction of FIG. 6(A), i.e. along the thickness direction.

(58) On the other hand, as shown in FIG. 6(B), a conventional R-T-B based alloy strip has less deposition of R.sub.2T.sub.14B phase crystal nuclei than in FIG. 6(A). In addition, the R.sub.2T.sub.14B phase crystals grow not only in the up-down direction but also in the left-right direction. Therefore, the lengths (widths) of the R.sub.2T.sub.14B phase columnar crystals in the direction perpendicular to the thickness direction are increased compared to FIG. 6(A). If the R-T-B based alloy strip has such a structure, it will not be possible to obtain alloy powder that is micronized and has excellent homogeneity of shape and size.

(59) <Method for Producing R-T-B Based Sintered Magnet>

(60) A preferred embodiment of the method for producing an R-T-B based sintered magnet will now be described. The method for producing an R-T-B based sintered magnet according to this embodiment comprises a melting step in which a molten R-T-B based alloy is prepared, a first cooling step in which the molten alloy is poured onto the roll surface of the cooling roll rotating in the circumferential direction, cooling the molten alloy by the roll surface to produce crystal nuclei, and solidifying at least a portion of the molten alloy, and a second cooling step in which the alloy containing crystal nuclei is further cooled to obtain an R-T-B based alloy strip, a grinding step in which the R-T-B based alloy strip is ground to obtain an R-T-B based alloy powder, a molding step in which the alloy powder is molded to form a compact, and a firing step in which the compact is fired to obtain an R-T-B based sintered magnet. Specifically, the method for producing an R-T-B based sintered magnet according to this embodiment can be carried out using an R-T-B based alloy strip obtained by the aforementioned method for producing, in the same manner as the method for producing an alloy strip described above from the melting step through to the second cooling step. The steps from the grinding step onward will therefore now be explained.

(61) There are no particular restrictions on the grinding method in the grinding step. The grinding can be carried out in the order of coarse grinding followed by fine grinding. Coarse grinding is preferably carried out in an inert gas atmosphere using, for example, a stamp mill, jaw crusher, Braun mill or the like. Hydrogen storage grinding may also be carried out, in which grinding is performed after hydrogen has been stored. By coarse grinding it is possible to prepare alloy powder with particle diameters of about several hundred m. The alloy powder prepared by coarse grinding is subjected to fine grinding to a mean particle diameter of 1 to 5 m, for example, using a jet mill or the like. Grinding of the alloy strip does not necessarily need to be carried out in two stages of coarse grinding and fine grinding, and may instead be carried out in a single step.

(62) In the grinding step, the sections of the grain boundary phases 4 such as the alloy strip R-rich phase sections preferentially undergo fracturing. Consequently, the particle diameters of the alloy powder depend on the spacing of the heterophase 4. The alloy strip to be used in the method for producing for this embodiment has lower variation in widths M of the R.sub.2T.sub.14B phase columnar crystals than in the prior art, as shown in FIG. 1, and therefore by grinding it is possible to obtain alloy powder having a small particle diameter and sufficiently reduced variation in size and shape.

(63) In the molding step, the alloy powder is molded in a magnetic field to obtain a compact. Specifically, first the alloy powder is packed into a die situated in an electromagnet. A magnetic field is then applied by the electromagnet and the alloy powder is pressed while orienting the crystal axes of the alloy powder. Molding is thus carried out in a magnetic field to prepare a compact. The molding in a magnetic field may be carried out in a magnetic field of 12.0 to 17.0 kOe, for example, at a pressure of about 0.7 to 1.5 ton/cm.sup.2.

(64) In the firing step, the compact obtained by the magnetic field molding is fired in a vacuum or in an inert gas atmosphere to obtain a sintered compact. The firing conditions are preferably set as appropriate for the conditions including the composition, the grinding method and the particle size. For example, the firing temperature may be set to 1000 C. to 1100 C. for a firing time of 1 to 5 hours.

(65) Since the R-T-B based sintered magnet obtained by the production method of this embodiment employs alloy powder comprising sufficiently micronized and highly homogeneous R.sub.2T.sub.14B phase crystals and an R-rich phase, it can yield an R-T-B based sintered magnet with a more micronized and homogeneous structure than the prior art. Consequently, the production method of this embodiment allows production of an R-T-B based sintered magnet having sufficiently high coercive force while maintaining residual flux density.

(66) The R-T-B based sintered magnet obtained by the process described above may also be subjected to aging treatment if necessary. By carrying out aging treatment, it is possible to further increase the coercive force of the R-T-B based sintered magnet. Aging treatment is preferably carried out in two stages, for example, under two different temperature conditions such as near 800 C. and near 600 C. Aging treatment under such conditions will tend to result in particularly excellent coercive force. When aging treatment is carried out in a single step, it is preferably at a temperature of near 600 C.

(67) The R-T-B based sintered magnet obtained in this manner has the following composition, for example. Specifically, the R-T-B based sintered magnet comprises R, B, Al, Cu, Zr, Co, O, C and Fe, the content ratio of each of the elements being R: 25 to 37 mass %, B: 0.5 to 1.5 mass %, Al: 0.03 to 0.5 mass %, Cu: 0.01 to 0.3 mass %, Zr: 0.03 to 0.5 mass %, Co: 3 mass % (not including 0 mass %), O: 0.5 mass % and Fe: 60 to 72 mass %. The composition of the R-T-B based sintered magnet will usually be the same as the composition of the R-T-B alloy strip.

(68) The R-T-B based sintered magnet may contain about 0.001 to 0.5 mass % of unavoidable impurities such as Mn, Ca, Ni, Si, Cl, S and F, in addition to the elements mentioned above. However, the content of these impurities is preferably less than 2 mass % and more preferably less than 1 mass % in total.

(69) The R-T-B based sintered magnet comprises an R.sub.2T.sub.14B phase as the main phase and an R-rich phase as the heterophase. Since the R-T-B based sintered magnet is obtained using alloy powder with a small particle diameter and low variation in particle diameter, it has increased structural homogeneity and sufficiently excellent coercive force.

(70) FIG. 7 is a schematic cross-sectional enlarged view showing a portion of a cross-section of the R-T-B based sintered magnet of this embodiment. The R-T-B based sintered magnet 100 preferably comprises at least Fe as a transition element (T), and more preferably it comprises a combination of Fe and a transition element other than Fe. Transition elements other than Fe include Co, Cu and Zr.

(71) The R-T-B based sintered magnet 100 preferably comprises at least one element selected from among Al, Cu, Ga, Zn and Ge. This will allow an R-T-B based sintered magnet 100 to be obtained with even higher coercive force. The R-T-B based sintered magnet 100 also preferably comprises at least one element selected from among Ti, Zr, Ta, Nb, Mo and Hf. By including such elements it is possible to suppress grain growth during firing, and further increase the coercive force of the R-T-B based sintered magnet 100.

(72) The rare earth element content of the R-T-B based sintered magnet 100 is preferably 25 to 37 mass % and more preferably 28 to 35 mass %, from the viewpoint of further increasing the magnetic properties. The B content of the R-T-B based sintered magnet 100 is preferably 0.5 to 1.5 mass % and more preferably 0.7 to 1.2 mass %.

(73) The rare earth elements include one or more elements selected from among scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb) and lutetium (Lu).

(74) The R-T-B based sintered magnet 100 may also contain a heavy rare earth element such as Dy, Tb or Ho as a rare earth element. In this case, the content of heavy rare earth elements in the total mass of the R-T-B based sintered magnet 100 is preferably no greater than 1.0 mass %, more preferably no greater than 0.5 mass % and even more preferably no greater than 0.1 mass %, as the total of the heavy rare earth elements. With the R-T-B based sintered magnet 100 of this embodiment, it is possible to obtain high coercive force even with such a low heavy rare earth element content.

(75) If the rare earth element content is less than 25 mass %, the amount of production of the R.sub.2T.sub.14B phase as the main phase of the R-T-B based sintered magnet 100 will be reduced, -Fe and the like having soft magnetism will be deposited more readily, and HcJ may potentially be reduced. If it is greater than 37 mass %, on the other hand, potentially the volume ratio of the R.sub.2T.sub.14B phase may be reduced and the residual flux density lowered.

(76) From the viewpoint of further increasing the coercive force, the R-T-B based sintered magnet 100 preferably contains a total of 0.2 to 2 mass % of at least one type of element selected from among Al, Cu, Ga, Zn and Ge. From the same viewpoint, the R-T-B based sintered magnet 100 also preferably comprises a total of 0.1 to 1 mass % of at least one element selected from among Ti, Zr, Ta, Nb, Mo and Hf.

(77) The content of transition elements (T) in the R-T-B based sintered magnet 100 is the remainder after the aforementioned rare earth elements, boron and added elements.

(78) When Co is included as a transition element, the content is preferably no greater than 3 mass % (not including 0), and more preferably 0.3 to 1.2 mass %. Co forms a phase similar to Fe, and including Co can increase the Curie temperature and corrosion resistance of the grain boundary phase.

(79) The oxygen content of the R-T-B based sintered magnet 100 is preferably 300-3000 ppm and more preferably 500-1500 ppm, from the viewpoint of achieving high levels for both magnetic properties and corrosion resistance. The nitrogen content of the R-T-B based sintered magnet 100 is 200 to 1500 ppm and preferably 500 to 1500 ppm, from the same viewpoint explained above. The carbon content of the R-T-B based sintered magnet 100 is 500 to 3000 ppm and preferably 800 to 1500 ppm, from the same viewpoint explained above.

(80) The crystal grains 120 of the R-T-B based sintered magnet 100 preferably comprise an R.sub.2T.sub.14B phase. On the other hand, the triple point regions 140 include a phase with a higher R content ratio than the R.sub.2T.sub.14B phase, based on mass compared to the R.sub.2T.sub.14B phase. The average value of the area of the triple point regions 140 in a cross-section of the R-T-B based sintered magnet 100 is no greater than 2 m.sup.2 and preferably no greater than 1.9 m.sup.2, as the arithmetic mean. Also, the standard deviation for the area distribution is no greater than 3 and preferably no greater than 2.6. Since the R-T-B based sintered magnet 100 thus has minimal segregation of the phase with a higher R content than the R.sub.2T.sub.14B phase, the area of the triple point regions 140 is low and the variation in area is also reduced. It is thus possible to maintain high levels for both Br and HcJ.

(81) The average value for the area of the triple point regions 140 in the cross-section, and the standard deviation for the area distribution, can be calculated in the following manner. First, the R-T-B based sintered magnet 100 is cut and the cut surface is polished. The polished surface image is observed with a scanning electron microscope. Image analysis is performed and the area of the triple point regions 140 is calculated. The arithmetic mean value for the calculated area is the mean area. Also, the standard deviation for the area of the triple point regions 140 can be calculated based on the area of each of the triple point regions 140 and their average value.

(82) The rare earth element content in the triple point regions 140 is preferably 80 to 99 mass %, more preferably 85 to 99 mass % and even more preferably 90 to 99 mass %, from the viewpoint of obtaining an R-T-B based sintered magnet with sufficiently high magnetic properties and sufficiently excellent corrosion resistance. From the same viewpoint, the rare earth element contents of each of the triple point regions 140 are preferably equal. Specifically, the standard deviation for the content distribution in the triple point regions 140 of the R-T-B based sintered magnet 100 is preferably no greater than 5, preferably no greater than 4 and more preferably no greater than 3.

(83) The mean particle diameter for the crystal grains 120 of the R-T-B based sintered magnet 100 is preferably 0.5 to 5 m and more preferably 2 to 4.5 from the viewpoint of further increasing the magnetic properties. The mean particle diameter can be calculated by performing image processing of the electron microscope image of a cross-section of the R-T-B based sintered magnet 100, measuring the particle diameters of the individual crystal grains 120, and taking the arithmetic mean of the measured values.

(84) The R-T-B based sintered magnet 100 comprises dendritic crystal grains 2 containing a R.sub.2T.sub.14B phase, and grain boundary regions 4 containing a phase with a higher R content than the R.sub.2T.sub.14B phase, and preferably it is obtained by molding and firing a ground product of an R-T-B based alloy strip having an average value of no greater than 3 m for the spacing between the phases with a higher R content than the R.sub.2T.sub.14B phase in a cross-section. Since such an R-T-B based sintered magnet 100 is obtained using a ground product that is sufficiently micronized and has a sharp particle size distribution, it is possible to obtain an R-T-B based sintered compact composed of fine crystal grains. In addition, since the phase with a higher R content than the R.sub.2T.sub.14B phase will be present in a higher proportion at the outer periphery than in the interior of the ground product, the state of dispersion of the phase with a higher R content than the R.sub.2T.sub.14B phase after sintering will tend to be more satisfactory. Thus, the structure of the R-T-B based sintered compact will be micronized and the homogeneity will be improved. It will thereby be possible to further increase the magnetic properties of the R-T-B based sintered compact.

(85) FIG. 8 is an illustration showing the internal structure of a motor comprising an R-T-B based sintered magnet 100 obtained by the production method described above. The motor 200 shown in FIG. 8 is a permanent magnet synchronous motor (SPM motor 200), comprising a cylindrical rotor 40 and a stator 50 situated on the inside of the rotor 40. The rotor 40 has a cylindrical core 42 and a plurality of R-T-B based sintered magnets 100 oriented with the N-poles and S-poles alternating along the inner peripheral surface of the cylindrical core 42. The stator 50 has a plurality of coils 52 provided along the outer peripheral surface. The coils 52 and R-T-B based sintered magnets 100 are arranged in a mutually opposing fashion.

(86) The SPM motor 200 is provided with an R-T-B based sintered magnet 100 in the rotor 40. The R-T-B based sintered magnet 100 exhibits high levels in terms of both high magnetic properties and excellent corrosion resistance. Thus, the SPM motor 200 comprising the R-T-B based sintered magnet 100 can continuously exhibit high output for prolonged periods.

(87) The embodiment described above is only a preferred embodiment of the invention, and the invention is in no way limited thereto. For example, the R-T-B based alloy strip of this embodiment had the crystal nuclei 1 of the R.sub.2T.sub.14B phase only on one side, but it may also have the crystal nuclei 1 on the other side of the R-T-B based alloy strip. In this case, both sides have crystal nuclei 1 such as shown in FIG. 1, and the columnar crystals 2 of the R.sub.2T.sub.14B phase extend in a radial fashion along the thickness direction from each of the crystal nuclei 1. Thus, an R-T-B based alloy strip having crystal nuclei 1 on both sides can be obtained by a twin-roll casting method in which two cooling rolls having the aforementioned concavoconvex pattern are aligned and molten alloy is cast between them.

EXAMPLES

(88) The nature of the invention will now be further explained through the following examples and comparative examples. However, the invention is not limited to the examples described below.

Example 1

(89) <Fabrication of Alloy Strip>

(90) An apparatus for production of an alloy strip as shown in FIG. 2 was used for a strip casting method by the following procedure. First, the starting compounds for each of the constituent elements were added so that the composition of the alloy strip had the elemental ratios (mass %) shown in Table 2, and heated to 1300 C. with a high-frequency melting furnace 10, to prepare a molten alloy 12 having an R-T-B based composition. The molten alloy 12 was poured onto the roll surface 17 of the cooling roll 16 rotating at a prescribed speed through a tundish. The cooling rate of the molten alloy 12 on the roll surface 17 was 1800 C. to 2200 C./sec.

(91) The roll surface 17 of the cooling roll 16 had a concavoconvex pattern comprising straight linear first recesses 32 extending along the rotational direction of the cooling roll 16, and straight linear second recesses 34 perpendicular to the first recesses 32. The average value H for the heights of the raised sections 36, the average value W for the spacings between the raised sections 36, and the surface roughness Rz, were as shown in Table 1. Measurement of the surface roughness Rz was carried out using a measuring apparatus by Mitsutoyo Corp. (trade name: SURFTEST).

(92) The alloy strip obtained by cooling with the cooling roll 16 was further cooled with a secondary cooling section 20 to obtain an alloy strip having an R-T-B based composition. The composition of the alloy strip was as shown in Table 2.

(93) <Evaluation of Alloy Strip>

(94) A SEM-BEI photograph was taken of a cross-section along the thickness direction of the obtained alloy strip (magnification: 350). The thickness of the alloy strip was determined from the photograph. The thickness was as shown in Table 1.

(95) In addition, SEM-BEI image photographs of cross-sections along the thickness direction of the alloy strip were for 15 visual fields on the casting surface side, the free surface side and at the center section, for a total of 45 SEM-BEI photographs (magnification: 1000). Using the photographs, 0.15 mm straight lines were drawn to a position 50 m on the center section side from the casting surface, a position 50 m on the center section side from the free surface, and to the center section. The values of D.sub.1, D.sub.2 and D.sub.3 were determined from the length of the straight line and the number of columnar crystals transected by the straight line.

(96) Incidentally, D.sub.1 is the average value for the lengths of the columnar crystals on the casting surface side in the direction perpendicular to the thickness direction, D.sub.2 is the average value for the lengths of the columnar crystals on the free surface side in the direction perpendicular to the thickness direction, and D.sub.3 is the average value for the lengths of the columnar crystal at the center section in the direction perpendicular to the thickness direction. The average value D.sub.AVE was calculated for D.sub.1, D.sub.2 and D.sub.3. In addition, the maximum for the lengths of the columnar crystals in the direction perpendicular to the thickness direction in the 45 photographs was recorded as D.sub.MAX. The measurement results were as shown in Table 1.

(97) Also, the 45 SEM-BEI image photographs were used to determine the percentage of the number of R-rich phases with lengths of up to 1.5 m on the straight line, with respect to the total number of R-rich phases through which the straight line crossed. The results were as shown in Table 1.

(98) <Fabrication of R-T-B Based Sintered Magnet>

(99) The alloy strip was then ground to obtain alloy powder with a mean particle diameter of 2.0 m. The alloy powder was packed into a die situated in an electromagnet, and molded in a magnetic field to produce a compact. The molding was accomplished by pressing at 1.2 ton/cm.sup.2 while applying a magnetic field of 15 kOe. The compact was then fired at 930 C. to 1030 C. for 4 hours in a vacuum and rapidly cooled to obtain a sintered compact. The obtained sintered compact was subjected to two-stage aging treatment at 800 C. for 1 hour and at 540 C. for 1 hour (both in an argon gas atmosphere), to obtain an R-T-B based sintered magnet for Example 1.

(100) <Evaluation of R-T-B Based Sintered Magnet>

(101) A B-H tracer was used to measure the Br (residual flux density) and HcJ (coercive force) of the obtained R-T-B based sintered magnet. The measurement results are shown in Table 1.

Examples 2 to 6, Examples 16 to 18

(102) Alloy strips for Examples 2 to 6 and Examples 16 to 18 were obtained in the same manner as Example 1, except that the roll surface of a cooling roll was worked to change the average value H for the heights of the raised sections, the average value W for the spacings between the raised sections and the surface roughness Rz, as shown in Table 1. The alloy strips of Examples 2 to 6 and Examples 16 to 18 were also evaluated in the same manner as Example 1. R-T-B based sintered magnets for Examples 2 to 6 and Examples 16 to 18 were fabricated in the same manner as Example 1, and evaluated. The results are shown in Table 1. FIG. 9 is an SEM-BEI photograph (magnification: 350) of a cross-section of the R-T-B based alloy strip of Example 5, along the thickness direction.

Examples 7 to 15 and Examples 19 to 31

(103) Alloy strips for Examples 7 to 15 and Examples 19 to 31 were obtained in the same manner as Example 1, except that the roll surface of a cooling roll was worked to change the average value for the heights of the raised sections, the average value for the spacings between the raised sections and the surface roughness Rz, as shown in Table 1, and the starting materials were changed to the compositions of the alloy strip as shown in Table 2. The alloy strips of Examples 7 to 15 and Examples 19 to 31 were also evaluated in the same manner as Example 1. Also, R-T-B based sintered magnets for Examples 7 to 15 and Examples 19 to 31 were fabricated in the same manner as Example 1, and evaluated. The results are shown in Table 1.

Comparative Example 1

(104) R-T-B based alloy strips for Comparative Example 1 and Comparative Example 2 were obtained in the same manner as Example 1, except that there were used cooling rolls having on the roll surface only straight linear first recesses extending in the rotational direction of the roll. These cooling rolls did not have second recesses. The average value H for the heights of the raised sections, the average value W for the spacings between the raised sections and the surface roughness Rz, for the cooling rolls, were determined in the following manner. Specifically, the cross-sectional structure near the roll surface was observed with a scanning electron microscope at the cut surface, when the cooling roll was cut on a plane parallel to the axial direction running through the axis of the cooling roll. The average value H for the heights of the raised sections is the arithmetic mean value for the heights of 100 raised sections, and the average value W for the spacings between the raised sections is the arithmetic mean value for the values of spacings between adjacent raised sections measured at 100 different locations.

(105) The alloy strip of Comparative Example 1 was evaluated in the same manner as Example 1. An R-T-B based sintered magnet for Comparative Example 1 was fabricated in the same manner as Example 1 and evaluated. The results are shown in Table 1.

Comparative Examples 2 and 3

(106) R-T-B based alloy strips for Comparative Examples 2 and 3 were obtained in the same manner as Example 1, except that the roll surface of a cooling roll was worked to change the average value H for the heights of the raised sections, the average value W for the spacings between the raised sections and surface roughness Rz, as shown in Table 1. The R-T-B based alloy strips of Comparative Examples 2 and 3 were also evaluated in the same manner as Example 1. R-T-B based sintered magnets for Comparative Examples 2 and 3 were fabricated in the same manner as Example 1 and evaluated. The results are shown in Table 1. FIG. 10 is an SEM-BEI photograph (magnification: 350) of a cross-section of the R-T-B based alloy strip of Comparative Example 3, along the thickness direction.

Comparative Example 4

(107) An R-T-B based alloy strip was obtained for Comparative Example 4 in the same manner as Example 1, except that there were used cooling rolls having only straight linear first recesses on the roll surfaces extending in the rotational direction of the rolls, and the starting materials were changed to the composition of the alloy strip as shown in Table 2. These cooling rolls did not have second recesses. The average value H for the heights of the raised sections, the average value W for the spacings between the raised sections and the surface roughness Rz, for the cooling rolls, were determined in the same manner as Comparative Example 1.

(108) The alloy strip of Comparative Example 4 was evaluated in the same manner as Example 1. An R-T-B based sintered magnet for Comparative Example 4 was fabricated in the same manner as Example 1 and evaluated. The results are shown in Table 1.

(109) TABLE-US-00001 TABLE 1 Cold roll surface Surface Raised section Raised section Cross section along thickness roughness height spacing Alloy strip direction of alloy strip Concavoconvex (Rz (mean value H) (mean value W) Thickness D.sub.AVE D.sub.MAX D.sub.1 D.sub.2 D.sub.3 pattern m m m mm m m m m m Example 1 perpendicular 4.2 7.0 66.0 0.30 2.95 3.91 2.96 3.05 2.84 Example 2 perpendicular 4.5 9.0 64.0 0.29 2.47 3.23 2.45 2.54 2.43 Example 3 perpendicular 3.9 11.6 60.0 0.27 2.36 2.75 2.30 2.42 2.37 Example 4 perpendicular 4.1 11.6 57.0 0.25 2.17 2.81 2.14 2.19 2.17 Example 5 perpendicular 4.4 13.0 54.0 0.23 2.00 2.59 1.97 2.00 2.04 Example 6 perpendicular 4.5 14.0 48.0 0.18 1.76 2.18 1.67 1.84 1.76 Example 7 perpendicular 4.3 8.5 65.0 0.23 2.05 2.45 1.95 2.12 2.08 Example 8 perpendicular 4.2 8.7 63.0 0.23 1.77 2.19 1.69 1.85 1.77 Example 9 perpendicular 4.4 9.2 67.0 0.23 1.56 1.94 1.49 1.63 1.55 Example 10 perpendicular 4.4 10.2 62.0 0.26 2.36 3.03 2.23 2.42 2.42 Example 11 perpendicular 4.5 10.6 64.0 0.24 2.41 3.14 2.28 2.48 2.48 Example 12 perpendicular 4.3 10.4 58.0 0.25 2.28 2.90 2.17 2.35 2.31 Example 13 perpendicular 4.3 9.9 57.0 0.23 2.32 2.88 2.21 2.43 2.33 Example 14 perpendicular 4.4 9.8 65.0 0.27 2.68 3.34 2.56 2.80 2.68 Example 15 perpendicular 4.4 10.7 57.0 0.23 2.22 2.78 2.12 2.30 2.23 Example 16 perpendicular 4.6 6.8 66.0 0.30 2.95 3.81 2.80 3.08 2.96 Example 17 perpendicular 4.7 14.2 47.0 0.17 1.50 1.92 1.48 1.50 1.53 Example 18 perpendicular 4.4 7.2 65.0 0.30 2.90 3.72 2.81 3.04 2.84 Example 19 perpendicular 4.2 6.8 65.0 0.31 3.08 3.98 2.96 3.14 3.09 Example 20 perpendicular 4.2 7.0 68.0 0.30 3.10 3.91 2.99 3.20 3.08 Example 21 perpendicular 4.3 6.9 66.0 0.29 2.98 3.91 2.88 3.09 3.00 Example 22 perpendicular 4.2 7.0 67.0 0.31 3.03 4.12 2.88 3.14 2.96 Example 23 perpendicular 4.1 7.1 64.0 0.30 3.10 4.09 2.93 3.12 3.10 Example 24 perpendicular 4.2 7.0 65.0 0.30 2.99 3.90 2.84 3.10 2.96 Example 25 perpendicular 4.2 7.2 66.0 0.30 2.95 3.80 2.82 3.02 2.94 Example 26 perpendicular 4.3 6.9 66.0 0.31 3.03 3.99 2.90 3.15 2.98 Example 27 perpendicular 4.2 7.1 67.0 0.28 2.90 3.95 2.84 3.10 3.02 Example 28 perpendicular 4.2 6.8 65.0 0.30 3.13 4.11 3.00 3.29 3.02 Example 29 perpendicular 4.2 7.2 68.0 0.30 3.09 3.95 2.96 3.22 3.02 Example 30 perpendicular 4.1 7.0 66.0 0.32 3.35 4.46 3.19 3.48 3.35 Example 31 perpendicular 4.2 7.1 67.0 0.29 3.23 3.37 3.11 3.39 3.27 Comp. Ex. 1 Rotating direction 2.9 5.8 126.1 0.29 4.32 5.52 4.02 4.57 4.38 Comp. Ex. 2 perpendicular 5.8 16.9 35.0 0.31 4.78 6.23 *1 4.66 5.12 Comp. Ex. 3 perpendicular 3.2 6.7 69.5 0.19 4.10 5.26 3.70 4.39 4.21 Comp. Ex. 4 Rotating direction 2.8 5.3 132.0 0.33 4.78 6.03 4.38 5.07 4.88 Percentage of Magnetic properties number of R-rich Br Hcj D.sub.2/D.sub.1 phases 1.5 m % (kG) (kOe) Example 1 1.03 91 14.0 16.4 Example 2 1.03 93 14.1 16.7 Example 3 1.05 95 13.9 17.5 Example 4 1.02 95 13.9 18.1 Example 5 1.02 97 13.8 18.8 Example 6 1.10 93 13.7 16.7 Example 7 1.09 93 13.8 17.5 Example 8 1.09 93 13.0 19.8 Example 9 1.09 94 12.6 20.6 Example 10 1.09 93 13.9 16.5 Example 11 1.09 93 14.0 16.7 Example 12 1.08 94 14.1 16.4 Example 13 1.10 92 14.0 16.3 Example 14 1.09 91 14.4 14.8 Example 15 1.08 94 13.2 18.2 Example 16 1.10 91 14.4 15.0 Example 17 1.01 98 13.5 18.0 Example 18 1.08 91 14.4 15.4 Example 19 1.06 92 14.0 16.6 Example 20 1.07 91 14.0 17.1 Example 21 1.07 93 13.9 19.1 Example 22 1.09 91 13.9 18.7 Example 23 1.06 91 14.4 15.1 Example 24 1.09 92 14.4 18.3 Example 25 1.07 88 14.5 17.1 Example 26 1.09 91 14.4 18.0 Example 27 1.09 90 13.5 17.9 Example 28 1.10 92 14.6 15.5 Example 29 1.09 92 14.6 15.6 Example 30 1.09 91 14.6 15.1 Example 31 1.09 91 14.7 14.4 Comp. Ex. 1 1.14 85 13.8 13.8 Comp. Ex. 2 unmeasurable 86 13.6 12.5 Comp. Ex. 3 1.19 82 13.8 14.0 Comp. Ex. 4 1.16 80 13.8 12.5 *1: Unmeasurable due to generation of chill crystals instead of columnar crystals.

(110) TABLE-US-00002 TABLE 2 Content based on mass of elements in R-T-B based alloy strip Nd Pr Dy Tb Co Cu Al Ga Zr B Fe Examples 1-6, 31.00 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 0.98 66.52 Examples 16-18, Comp. Exs. 1-3 Example 7 32.50 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 0.98 65.02 Example 8 34.00 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 0.98 63.52 Example 9 34.70 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 0.98 62.82 Example 10 25.00 6.00 0.00 0.00 0.50 0.10 0.20 0.10 0.20 1.00 66.90 Example 11 31.10 0.00 0.10 0.00 1.00 0.10 0.20 0.10 0.10 1.02 66.28 Example 12 28.10 3.10 0.00 0.00 1.10 0.10 0.20 0.10 0.10 0.98 66.22 Example 13 22.40 8.90 0.00 0.00 1.00 0.10 0.20 0.00 0.10 0.99 66.31 Example 14 24.10 6.30 0.00 0.00 0.50 0.10 0.30 0.00 0.20 0.98 67.52 Example 15 28.30 5.80 0.00 0.00 0.50 0.20 0.10 0.30 0.20 1.03 63.57 Example 19 31.10 0.00 0.10 0.00 1.00 0.10 0.20 0.10 0.10 1.02 66.28 Example 20 30.00 0.00 1.00 0.00 1.00 0.10 0.20 0.00 0.20 1.00 66.50 Example 21 30.90 0.00 0.30 0.00 1.00 0.10 0.20 0.10 0.10 1.02 66.28 Example 22 22.40 8.40 0.50 0.00 1.00 0.10 0.20 0.00 0.10 0.99 66.31 Example 23 24.00 6.30 0.00 0.10 0.50 0.10 0.30 0.00 0.20 0.98 67.52 Example 24 28.70 0.00 0.80 0.00 0.50 0.08 0.20 0.00 0.20 0.88 68.64 Example 25 29.10 0.00 0.40 0.00 0.50 0.03 0.20 0.00 0.20 0.90 68.67 Example 26 28.80 0.00 0.70 0.00 0.50 0.08 0.20 0.00 0.25 0.90 68.57 Example 27 34.00 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 1.03 63.47 Example 28 29.50 0.00 0.00 0.00 0.50 0.10 0.20 0.00 0.06 0.90 68.74 Example 29 29.50 0.00 0.00 0.00 0.50 0.20 0.20 0.00 0.20 0.91 68.49 Example 30 28.30 0.00 0.00 0.00 1.00 0.10 0.20 0.00 0.20 1.10 69.10 Example 31 28.30 0.00 0.00 0.00 2.80 0.10 0.20 0.00 0.20 1.00 67.40 Comp. Ex. 4 25.00 6.00 0.00 0.00 0.50 0.10 0.20 0.10 0.20 1.00 66.90 Units of values in the table are mass %. Values for Fe include unavoidable impurities.

(111) The results shown in Table 1 confirmed that the R-T-B based sintered magnets of Examples 1 to 31 have excellent coercive force.

(112) [Structural Analysis of R-T-B Based Sintered Magnets]

(113) (Area and Standard Deviation for Triple Point Regions)

(114) For the R-T-B based sintered magnet of Example 10 there was used an electron beam microanalyzer (EPMA: JXA8500F Model FE-EPMA), and element map data were collected. The measuring conditions were: an acceleration voltage of 15 kV, an irradiation current of 0.1 A and a count-time: of 30 msec, the data acquisition region was X=Y=51.2 m, and the number of data points was X=Y=256 (0.2 m-step). In the element map data, first triple point regions surrounded by 3 or more crystal grains are colored black, and by image analysis thereof, the average value for the area of the triple point regions and the standard deviation for the area distribution were calculated. FIG. 12 is a diagram showing element map data for the rare earth sintered magnet of Example 10, with the triple point regions indicated in black.

(115) The EPMA was used for structural observation of the R-T-B based sintered magnets of Examples 10 to 15 and Comparative Example 4 in the same manner as the R-T-B based sintered magnet of Example 10. FIG. 13 is a diagram showing element map data for the R-T-B based sintered magnet of Comparative Example 4, with the triple point regions indicated in black.

(116) Image analysis was performed for Examples 10 to 15 and Comparative Example 4 in the same manner as Example 10, and the average value for the area of the triple point regions and the standard deviation for the area distribution were calculated. The results are shown in Table 3. As shown in Table 3, the R-T-B based sintered magnets of Examples 10 to 15 had sufficiently smaller values for the average value and standard deviation for the area of the triple point regions, compared to Comparative Example 4. These results confirmed that in Examples 10 to 15, segregation of the phase with a higher R content than the R.sub.2T.sub.14B phase was inhibited.

(117) (Mean Particle Diameter)

(118) In addition, using a similar electron microscope observation image, the shapes of the R.sub.2T.sub.14B phase crystal grains were discerned by image analysis, the diameters of each of the individual crystal grains were determined, and the arithmetic mean value was obtained. This was recorded as the mean particle diameter of the R.sub.2T.sub.14B phase crystal grains. The results are shown in Table 3.

(119) (Rare Earth Element Content of Triple Point Regions)

(120) EPMA was used to determine the rare earth element content of the triple point regions of the R-T-B based sintered magnets of Examples 10 to 15 and Comparative Example 4, based on mass. The measurement was conducted for 10 triple point regions, and the range and standard deviation for the rare earth element content was determined. The results are shown in Table 3.

(121) (Oxygen, Nitrogen and Carbon Contents)

(122) A common gas analysis apparatus was used for gas analysis of the R-T-B based sintered magnets of Examples 10 to 15 and Comparative Example 4, and the oxygen, nitrogen and carbon contents were determined. The results are shown in Table 3.

(123) TABLE-US-00003 TABLE 3 Rare earth Mean Triple point elements of triple particle region area point regions Oxygen Nitrogen Carbon diameter Mean value Content content content content (m) (m.sup.2) S.D. (mass %) S.D. (ppm) (ppm) (ppm) Example 10 3.32 1.2 1.1 92-98 2.4 590 560 1100 Example 11 3.25 1.8 2.6 91-98 2.7 890 820 950 Example 12 3.43 1.5 2.3 92-98 2.5 780 780 1020 Example 13 3.22 1.7 2.1 91-98 2.8 650 870 980 Example 14 4.31 1.3 1.5 92-98 2.1 530 680 1440 Example 15 3.86 1.9 1.7 93-98 2.6 1420 1010 1380 Comp. Ex. 4 3.65 3.4 7.1 82-98 5.7 800 760 1380

(124) A shown in Tables 1 and 3, although Example 10 and Comparative Example 4 both used alloy powder having about the same mean particle diameter, the R-T-B sintered magnet obtained in Example 10 had a higher HcJ value. This is presumably because the R-T-B based sintered magnet of Example 10 not only had a finer crystal grain particle diameter, but also had more uniform particle diameters and shapes of the crystal grains, and therefore reduced segregation of the triple point regions.

INDUSTRIAL APPLICABILITY

(125) According to the invention it is possible to provide an alloy strip that can increase the coercive force of an R-T-B based sintered magnet. It is also possible to provide an R-T-B based sintered magnet having sufficiently excellent coercive force, as well as a method for producing it.

EXPLANATION OF SYMBOLS

(126) 1: Crystal nuclei, 2: columnar crystal, 4: grain boundary phase (heterophase), 10: high-frequency melting furnace, 12: molten alloy, 14: tundish, 16: cooling roll, 17: roll surface, 18: alloy strip, 19: gas tube, 19a: gas blow hole, 20: secondary cooling section, 32, 34: recesses, 36: raised section, 100: R-T-B based sintered magnet, 120: crystal grain, 140: triple point region (grain boundary region), 40: rotor, 42: core, 50: stator, 52: coil, 200: motor.