HOT-DEFORMED MAGNET, METHOD FOR PRODUCING RAW MATERIAL POWDER FOR HOT-DEFORMED MAGNET, AND METHOD FOR PRODUCING HOT-DEFORMED MAGNET
20190337051 ยท 2019-11-07
Assignee
Inventors
- Yoshiyuki Nakazawa (Wako-shi, JP)
- Ryutaro Kato (Wako-shi, JP)
- Yasutaka Shintani (Wako-shi, JP)
- Haruhiko Shimizu (Wako-shi, JP)
- Takeshi Okuno (Wako-shi, JP)
Cpc classification
B22F2009/048
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
C22C38/002
CHEMISTRY; METALLURGY
B22F2009/048
PERFORMING OPERATIONS; TRANSPORTING
B22F2301/355
PERFORMING OPERATIONS; TRANSPORTING
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
C22C38/005
CHEMISTRY; METALLURGY
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B22F1/142
PERFORMING OPERATIONS; TRANSPORTING
B22F1/142
PERFORMING OPERATIONS; TRANSPORTING
International classification
B22F1/00
PERFORMING OPERATIONS; TRANSPORTING
B22F9/04
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A hot-deformed magnet is obtained by quenching and solidifying a melt of an alloy containing a rare earth element (RE), Fe, and B as main components by a super quenching method using a rotating roll; preparing an alloy powder in an amorphous structure state or an amorphous-microcrystalline mixed structure state; subjecting the alloy powder to a rapid heat treatment in a falling-type heating furnace so as to obtain a raw material powder; hot-forming the raw material powder so as to densify the raw material powder to near true density and form a hot-formed compact; and subjecting the hot-formed compact to uniaxial hot plastic working to orient crystals.
Claims
1. A method for producing a raw material powder for a hot-deformed magnet, the method comprising steps of: (i) preparing an alloy powder in an amorphous structure state or an amorphous-microcrystalline mixed structure state, the step (i) comprising quenching and solidifying a melt of an alloy containing a rare earth element (RE), Fe, and B as main components by a super quenching method using a rotating roll; and (ii) subjecting the alloy powder to a rapid heat treatment in a falling-type heating furnace so as to obtain a raw material powder.
2. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein: conditions for the rapid heat treatment in the falling-type heating furnace include that: a temperature elevation rate is 400 C./minute or more, a heating temperature is equal to or higher than a crystallization onset temperature of the alloy powder and is 600 C. to 800 C., and an atmosphere inside the falling-type heating furnace is a vacuum or an inert atmosphere; and the rapid heat treatment is performed at least once under these conditions.
3. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein a heating zone of the falling-type heating furnace has a length of 0.5 m or more, and a furnace core into which the alloy powder falls extends substantially in a vertical direction or is slanted within 5 with respect to the vertical direction.
4. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein 50% or more of the raw material powder after the rapid heat treatment is crystallized, and an oxygen concentration of the raw material powder or an oxygen concentration of a hot-deformed magnet produced by using the raw material powder is 3000 ppm or less.
5. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein the alloy containing the rare earth element (RE), Fe, and B as main components is represented by a compositional formula, RE.sub.x(Fe, Co).sub.100-xB.sub.yM.sub.z, where: RE represents a rare earth element that contains 90 atom % or more of one or both of Pr and Nd, and 0 atom % or more and 10 atom % or less of at least one element selected from Y and lanthanoid series elements other than Pr and Nd, M represents at least one element selected from the group consisting of Al, Si, Ti, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Hf, Ta, W, Pt, Pb, Au, and Ag, and compositional ratios x, y, and z satisfy 12x16, 4y7, and 0.01z5.
6. A method for producing a hot-deformed magnet, comprising: subjecting the raw material powder obtained by the method according to claim 1 to hot-forming to densify the raw material powder to substantially true density so as to form a hot-formed compact; and subjecting the hot-formed compact to uniaxial hot plastic working to orient crystals.
7. A hot-deformed magnet produced by the method according to claim 6.
8. The hot-deformed magnet according to claim 7, wherein coarse crystal grains having a crystal grain size of 0.5 m or more are present at an area ratio of 10% or less.
9. The hot-deformed magnet according to claim 7, wherein Dy or Tb is not contained, and a product of a residual magnetic flux density (kG) and a coercive force (kOe) is 250 or more.
10. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein the step (i) comprises quenching and solidifying the melt of the alloy on a surface of the rotating roll to produce a strip of solidified alloy and pulverizing the strip.
11. The method for producing a raw material powder for a hot-deformed magnet according to claim 1, wherein the step (ii) comprises heating the alloy powder while the alloy powder falls down by free fall inside the heating furnace.
12. The method for producing a raw material powder for a hot-deformed magnet according to claim 4, wherein the raw material powder has 50% or more of degree of crystallinity.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The advantages of the disclosure will become apparent in the following description taken in conjunction with the following drawings.
[0017]
[0018]
[0019]
[0020]
[0021]
[0022]
[0023]
[0024]
[0025]
DETAILED DESCRIPTION
1. Powder Forming Step
[0026]
[0027] The alloy contains RE-FeB as main components (RE represents a rare earth element), and the following alloy is used. The alloy is represented by a compositional formula, RE.sub.x(Fe, Co).sub.100-xB.sub.yM.sub.z, where RE represents a rare earth element that contains 90 atom % or more of one or both of Pr and Nd, and 0 atom % or more and 10 atom % or less of at least one element selected from Y and lanthanoid series elements other than Pr and Nd, M represents at least one element selected from the group consisting of Al, Si, Ti, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Hf, Ta, W, Pt, Pb, Au, and Ag, and compositional ratios x, y, and z satisfy 12x16, 4y7, and 0.01z5.
2. Rapid Heating Step
[0028]
[0029] In the rapid heating step, the interior of the metal tube 21 is vacuumed or substituted by an inert atmosphere such as Ar gas, and is heated to 600 C. to 800 C. The powder 4 is injected into the metal tube 21 by using a hopper (not illustrated in the drawings) from an upper end opening of the metal tube 21. The powder 4 is rapidly heated as the powder 4 falls inside the metal tube 21.
[0030] The length of the heating zone in which the powder 4 is heated inside the metal tube 21 is at least 0.5 m and is, for example, several meters. In addition, the furnace core inside the metal tube 21 into which the alloy powder falls is installed to extend in a vertical direction or may be slanted within 5 with respect to the vertical direction. The powder 4 falls onto the recovery box 20 by free fall inside the metal tube 21 in, for example, about 5 seconds. The temperature elevation rate of the powder 4 in the metal tube 21 is preferably 400 C./minute or more.
[0031]
3. Densifying Step
[0032] Next, as illustrated in
4. Plastic Working Step
[0033] Next, as illustrated in
EXAMPLES
[0034] The present disclosure will now be described in detail through more specific examples.
1. Experimental Example 1 (Regarding the Influence of the Heating Temperature)
[0035] An alloy ribbon (Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6) prepared by a super quenching method using a rotating roll was roughly pulverized to prepare a raw material powder. A hot-deformed magnet was prepared by hot-forming this raw material powder at 650 C. by using a hot pressing machine until the density was near the true density, and then uniaxially hot-plastic-working the hot-formed compact at 700 C. until the reduction reached 70% (Comparative Example 1). The reduction is defined as follows: (1height after plastic working/height before plastic working)100%.
[0036] In contrast, a hot-deformed magnet was prepared by subjecting a raw material powder having the composition of Comparative Example 1 above to a rapid heat treatment using the falling-type heating furnace illustrated in
TABLE-US-00001 TABLE 1 Rapid heat treatment Powder conditions crystallinity Magnetic properties after hot Coarse Heating Heated after rapid deforming grain Raw material powder temperature length heating Br iHc Hk/iHc Br area components ( C.) (m) (%) (kG) (kOe) (%) iHc (%) Example 1 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 500 5 0 12.37 20.08 79.9 248 19.5 Example 2 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 550 5 3.0 12.38 20.05 85.4 248 19.4 Example 3 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 600 5 52.4 12.77 19.65 88.7 251 17.2 Example 4 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 650 5 99.9 13.08 21.13 90.6 276 7.3 Example 5 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 675 5 100.0 13.16 21.30 91.7 280 6.5 Example 6 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 700 5 100.0 13.23 21.13 92.1 280 3.9 Example 7 Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 725 5 100.0 13.32 20.34 84.9 271 3.4 Comparative Nd.sub.10.5Pr.sub.3.6Fe.sub.77.4Co.sub.2.5Ga.sub.0.5B.sub.5.6 0 12.41 20.59 78.4 256 19.5 Example 1
[0037] For the hot-deformed magnets of Examples 1 to 7 and Comparative Example 1 prepared as described above, the powder crystallinity defined as the difference in heat of crystallization obtained through a differential scanning calorimetry was investigated. In addition, a superconducting-type vibrating sample magnetometer (VSM-5T produced by Riken Denshi Co., Ltd.) was used to evaluate magnetic properties. Furthermore, a resin-embedded specimen of the hot-deformed magnet was mirror-polished and surface-etched to make the structure prominent, and then the structure was observed by using a FE-SEM (S-4300SE/N produced by Hitachi High-Technologies Corporation). The coarse grain (average grain diameter: 0.5 m or more) existing area was calculated from the observed structure image by using image analysis software. The results are indicated in Table 1.
[0038]
2. Experimental Example 2 (Regarding the Influence of the Heated Length)
[0039] An alloy ribbon (Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6) prepared by a super quenching method using a rotating roll was roughly pulverized to prepare a raw material powder. A hot-deformed magnet was prepared by hot-forming the raw material powder at 650 C. by using a hot pressing machine until the density was near the true density, and then uniaxially hot-plastic-working the hot-formed compact at 750 C. until the reduction reached 70% (Comparative Example 2).
[0040] In contrast, a hot-deformed magnet was prepared by subjecting the raw material powder having the composition of Comparative Example 2 above to a rapid heat treatment using the falling-type heating furnace illustrated in
TABLE-US-00002 TABLE 2 Rapid heat treatment Powder conditions crystallinity Magnetic properties after hot Coarse Heating Heated after rapid deforming grain Raw material powder temperature length heating Br iHc Hk/iHc Br area components ( C.) (m) (%) (kG) (kOe) (%) iHc (%) Example 8 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 0.5 3.3 13.20 19.61 92.8 259 16.8 Example 9 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 1.0 51 13.55 19.99 93.0 271 9.2 Example 10 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 1.5 76.7 13.70 19.97 94.0 274 6.2 Example 11 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 2.5 99.7 13.96 19.98 95.3 279 3.1 Example 12 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 5.0 100 13.94 19.94 95.0 278 2.4 Example 13 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 700 0.5 4.1 13.30 19.58 92.8 260 16.0 Example 14 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 750 1.0 77.8 13.68 19.93 94.6 273 5.8 Example 15 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 750 1.5 92.9 14.04 19.82 94.5 278 3.7 Example 16 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 750 2.5 99.6 14.09 19.65 94.1 277 1.7 Example 17 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 750 5.0 100 14.10 19.36 93.5 273 0.9 Example 18 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 800 0.5 4.8 13.35 19.62 92.9 262 14.1 Example 19 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 800 1.0 99.7 13.62 20.00 93.5 272 2.6 Example 20 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 800 1.5 98 13.94 19.55 94.4 273 1.2 Example 21 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 800 2.5 99.9 14.00 19.40 93.4 272 0.4 Example 22 Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 800 5.0 100 13.85 19.02 92.5 263 0 Comparative Nd.sub.10.5Pr.sub.3.5Fe.sub.77.2Co.sub.2.5Ga.sub.0.7B.sub.5.6 0 13.23 19.50 92.8 258 17.2 Example 2
[0041] For the hot-deformed magnets of Comparative Example 2 and Examples 8 to 22 prepared as above, the powder crystallinity, the magnetic properties, and the coarse grain existing area were investigated by the same method as in Experimental Example 1 (regarding the influence of the heating temperature). The results are indicated in Table 2.
[0042] As apparent from
3. Experimental Example 3 (Regarding the Influence of the Oxygen Concentration)
[0043] An alloy ribbon (Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6) prepared by a super quenching method using a rotating roll was roughly pulverized to prepare a raw material powder. Here, the powder grain size was changed during rough pulverization of the alloy ribbon so that raw material powders with different oxygen concentrations were obtained as illustrated in Table 3 (Comparative Examples 3 to 5). Each of these raw material powders was hot-formed at 650 C. by using a hot pressing machine until the density was near the true density, and the resulting hot-formed compact was uniaxially hot-plastic-worked at 700 C. until the reduction reached 70% so as to obtain hot-deformed magnets of Comparative Examples 3 to 5.
[0044] In contrast, hot-deformed magnets were prepared by subjecting each of the raw material powders respectively having the compositions of Comparative Examples 3 to 5 above to a rapid heat treatment using the falling-type heating furnace illustrated in
TABLE-US-00003 TABLE 3 Oxygen concentration Rapid heat treatment conditions (wt %) Magnetic Heating In-fumace Powder properties after tem- Heated oxygen after hot deforming Raw material powder perature length concentration rapid After hot Br iHc Br components ( C.) (m) Atmosphere (ppm) heating deforming (kG) (kOe) iHc Example 23 Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 700 5 Injected simultaneously 737 0.541 0.561 11.10 12.30 137 with Ar flow Example 24 Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 700 5 Injected 1 minute 312 0.282 0.294 12.93 16.98 220 after Ar flow Example 25 Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 700 5 Injected 5 minutes 209 0.214 0.220 13.06 18.38 240 after Ar flow Example 26 Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 700 5 Injected 10 minutes 84 0.112 0.120 13.09 19.90 260 after Ar flow Example 27 Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 Ar flow after 3 0.052 0.052 13.08 21.41 280 vacuum substitution Comparative Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 0.173 0.175 12.56 16.91 212 Example 3 Comparative Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 0.058 0.070 12.59 19.68 248 Example 4 Comparative Nd.sub.10.5Pr.sub.3.5Fe.sub.77Co.sub.3Ga.sub.0.4B.sub.5.6 0.044 0.050 12.55 20.26 254 Example 5
[0045] For the hot-deformed magnets of Comparative Examples 3 to 5 and Examples 23 to 27 prepared as above, the magnetic properties were investigated by the same method as in Experimental Example 1 (regarding the influence of the heating temperature). In addition, for Comparative Examples 3 to 5 and Examples 23 to 27, the oxygen concentrations in the raw material powders after the rapid heating and in the compacts after the hot plastic working were investigated. The results are indicated in Table 3.
[0046] According to
4. Experimental Example 4 (Regarding the Influence of the Components)
[0047] The alloys having compositions with various RE contents as in Examples 28 to 33 and Comparative Examples 6 to 11 indicated in Table 4 were prepared into alloy ribbons by a super quenching method using a rotating roll, and the alloy ribbons were roughly pulverized to prepare raw material powders. Each of the raw material powders of Comparative Examples 6 to 11 was hot-formed at 650 C. by using a hot pressing machine until the density was near the true density, and the resulting hot-formed compact was uniaxially hot-plastic-worked at 750 C. until the reduction reached 70% so as to obtain hot-deformed magnets of Comparative Examples 6 to 11.
[0048] In contrast, hot-deformed magnets of Examples 28 to 33 were prepared by subjecting the raw material powders of Examples 28 to 33 to a rapid heat treatment using the falling-type heating furnace illustrated in
TABLE-US-00004 TABLE 4 Rapid heat treatment conditions Magnetic properties after hot Coarse Constituent components Heating Heated deforming grain RE temperature length Br iHc Hk/iHc Br area Nd Pr Nd + Pr Fe Co Ga B ( C.) (m) (kG) (kOe) (%) iHc (%) Example 28 9.6 3.1 12.7 78.7 2.5 0.5 5.6 700 5 14.80 17.06 97.5 252 0 Example 29 10 3.3 13.3 78.1 2.5 0.5 5.6 700 5 14.02 19.51 95.4 274 0.6 Example 30 10.3 3.4 13.7 77.7 2.5 0.5 5.6 700 5 13.61 20.41 93.8 278 1.5 Example 31 10.5 3.6 14.1 77.3 2.5 0.5 5.6 700 5 13.23 21.13 93.1 280 2.4 Example 32 10.9 3.6 14.5 76.9 2.5 0.5 5.6 700 5 12.57 22.02 92.3 277 3.3 Example 33 11.3 3.7 15.0 76.4 2.5 0.5 5.6 700 5 11.92 22.56 90.5 269 4.0 Comparative 9.6 3.1 12.7 78.7 2.5 0.5 5.6 14.21 16.63 95.1 236 13.2 Example 6 Comparative 10 3.3 13.3 78.1 2.5 0.5 5.6 13.18 18.97 92.1 250 14.4 Example 7 Comparative 10.3 3.4 13.7 77.7 2.5 0.5 5.6 13.06 19.40 89.9 253 15.8 Example 8 Comparative 10.5 3.6 14.1 77.3 2.5 0.5 5.6 12.41 20.59 89.1 256 17.2 Example 9 Comparative 10.9 3.6 14.5 76.9 2.5 0.5 5.6 11.68 21.58 88.0 252 18.7 Example 10 Comparative 11.3 3.7 15.0 78.9 2.5 0.5 5.6 11.17 22.05 87.2 246 20.0 Example 11
[0049] For the hot-deformed magnets of Comparative Examples 28 to 33 and Comparative Examples 6 to 11 prepared as above, the magnetic properties and the coarse grain existing area were investigated by the same method as in Experimental Example 1 (regarding the influence of the heating temperature). The results are indicated in Table 4.
[0050] According to
[0051] The present disclosure is applicable to permanent magnets used in motors and the like.