METHOD FOR MANUFACTURING SOFT MAGNETIC IRON POWDER
20200001369 ยท 2020-01-02
Assignee
Inventors
- Makoto NAKASEKO (Tokyo, JP)
- Naomichi Nakamura (Tokyo, JP)
- Mineo Muraki (Tokyo, JP)
- Takuya TAKASHITA (Tokyo, JP)
Cpc classification
B22F2009/0888
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
C22C33/0257
CHEMISTRY; METALLURGY
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B22F1/08
PERFORMING OPERATIONS; TRANSPORTING
C22C33/0257
CHEMISTRY; METALLURGY
International classification
B22F9/08
PERFORMING OPERATIONS; TRANSPORTING
Abstract
Provided is a method for manufacturing soft magnetic iron powder.
A method for manufacturing soft magnetic iron powder, the method including ejecting high-pressure water to collide with a molten metal stream falling vertically downward, breaking up the molten metal stream into metal powder, and cooling the metal powder, in which, when a falling rate of the molten metal stream per unit time is defined as Qm (kg/min) and an ejection rate of high-pressure water per unit time is defined as Qaq (kg/min), a mass ratio (Qaq/Qm) is 50 or more, and a total content of ferrous constituents (Fe, Ni, and Co) is 76 at % or more.
Claims
1. A method for manufacturing soft magnetic iron powder, the method comprising ejecting high-pressure water to collide with a molten metal stream falling vertically downward, breaking up the molten metal stream into metal powder, and cooling the metal powder, wherein when a falling rate of the molten metal stream per unit time is defined as Qm (kg/min) and an ejection rate of the high-pressure water per unit time is defined as Qaq (kg/min), a mass ratio (Qaq/Qm) is 50 or more, and a total content of ferrous constituents (Fe, Ni, and Co) is 76 at % or more.
2. The method for manufacturing soft magnetic iron powder according to claim 1, wherein an ejection pressure of the high-pressure water is 25 MPa to 60 MPa, and the total content of the ferrous constituents is 78 at % or more.
3. The method for manufacturing soft magnetic iron powder according to claim 1, wherein a temperature of the high-pressure water is 20 C. or lower, and the total content of the ferrous constituents is 80 at % or more.
4. A method for manufacturing soft magnetic iron powder, the method comprising ejecting high-pressure water to collide with a molten metal stream falling vertically downward, breaking up the molten metal stream into metal powder, and cooling the metal powder, wherein when a falling rate of the molten metal stream per unit time is defined as Qm (kg/min) and an ejection rate of the high-pressure water per unit time is defined as Qaq (kg/min), a mass ratio (Qaq/Qm) is controlled on the basis of a correlation between the mass ratio (Qaq/Qm) and an amorphous material fraction of soft magnetic iron powder to achieve a desired amorphous material fraction, and a total content of ferrous constituents (Fe, Ni, and Co) is 76 at % or more.
5. The method for manufacturing soft magnetic iron powder according to claim 4, wherein the mass ratio is controlled by controlling a diameter of a teeming nozzle bore, through which the molten metal stream falls downward, and/or by controlling an ejection pressure of the high-pressure water.
6. The method for manufacturing soft magnetic iron powder according to claim 2, wherein a temperature of the high-pressure water is 20 C. or lower, and the total content of the ferrous constituents is 80 at % or more.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0019]
[0020]
[0021]
[0022]
[0023]
[0024]
[0025]
[0026]
DETAILED DESCRIPTION OF EMBODIMENTS OF THE INVENTION
[0027] Hereafter, embodiments of the present invention will be described. Here, the present invention is not limited to the embodiments below.
[0028]
[0029] In
[0030] As described in detail below with reference to
[0031] In addition, as indicated in
[0032]
[0033] As indicated in
[0034]
[0035] Here, in contrast, it is clarified that, in the case where the ejection pressure is 25 MPa, it is possible to achieve a very high amorphous material fraction by controlling the mass ratio (Qaq/Qm) to be 50 or more, even when the total content of ferrous constituents is 78 at %. From these results, it is clarified that it is possible to markedly increase the amorphous material fraction of soft magnetic iron powder by increasing ejection pressure, even in the case where the total content of ferrous constituents is 78 at % or more.
[0036] The reason why it is possible to achieve, even in the case where the total content of ferrous constituents is high, a markedly high amorphous material fraction by increasing ejection pressure is considered to be because it is possible to manufacture soft magnetic iron powder by cooling metal powder while destroying a vapor film.
[0037] Here, it is preferable that the upper limit of the ejection pressure be 60 MPa or less, because the upper limit of industrial pipework is generally 60 MPa, and because it is difficult to manufacture a valve through which a large amount of water is caused to flow in the case where the ejection pressure is more than 60 MPa. In addition, it is preferable that the total content of ferrous constituents be 82.5 at % or less in the case of the method utilizing ejection pressure, because it is possible to markedly increase the amorphous material fraction by controlling the ejection pressure to be 25 MPa to 60 MPa only in the case where the total content of ferrous constituents is 82.5 at % or less.
[0038]
[0039] In the case of
[0040] As indicated in
[0041] In addition, it is preferable that the total content of ferrous constituents be 82.5 at % or less in the case of the method utilizing water temperature control, because it is possible to markedly increase the amorphous material fraction by controlling the water temperature to be 20 C. or lower only in the case where the total content of ferrous constituents is 82.5 at % or less.
[0042] In addition, also in the case of
[0043] As described above, either by decreasing the temperature of the high-pressure water, or by increasing the ejection pressure of the high-pressure water, it is possible to markedly increase the amorphous material fraction of soft magnetic iron powder in the case where the mass ratio (Qaq/Qm) is 50 or more. As described above, although difficulty in markedly increasing the amorphous material fraction of soft magnetic iron powder increases with an increase in the total content of ferrous constituents, it is possible to markedly increase the amorphous material fraction of soft magnetic iron powder by a combination of a method in which the temperature of the high-pressure water is decreased and a method in which the ejection pressure of the high-pressure water is increased, even in the case where the total content of ferrous constituents is very high. Here, the expression the total content of ferrous constituents is very high refers to a case where the total content of ferrous constituents is 80 at % or more. In addition, it is preferable that the total content of ferrous constituents be 85.0 at % or less in the case of the method utilizing both water temperature control and ejection pressure control, because it is possible to markedly increase the amorphous material fraction by controlling water temperature to be 20 C. or lower and by controlling ejection pressure to be 25 MPa to 60 MPa only in the case where the total content of ferrous constituents is 85.0 at % or less.
[0044] Hereafter, a method for controlling the mass ratio (Qaq/Qm) will be described. To control the mass ratio (Qaq/Qm), it is necessary to control the flow rate of a high-pressure water pump or the flow rate of the molten metal stream. In the case where the ejection pressure of the high-pressure water is fixed, since it is difficult to change the flow rate of the high-pressure water without changing cooling water-ejecting nozzle bodies, it is cumbersome to change the flow rate of the high-pressure water pump. Therefore, it is preferable that the mass ratio (Qaq/Qm) be controlled by controlling the flow rate of the molten metal stream. Specifically, the controlling method is as follows.
[0045] First, there is a method in which, as illustrated in
[0046] Specific means for controlling the teeming nozzle bore diameter will be described with reference to
[0047] Hereafter, control of the temperature of the high-pressure water will be described with reference to
[0048] It is possible to control the temperature of the cooling water to be a desired temperature by checking the temperature of the water in the cooling-water tank with a thermometer (unillustrated) and by using the cooling water-temperature controller 16.
[0049] Hereafter, a method for controlling the ejection pressure of the high-pressure water will be described. It is possible to control the ejection pressure by controlling the rotation speed of the high-pressure pump through inverter control. In addition, in the case where the flow rate of the water is controlled with a constant ejection pressure, it is possible to perform the control by changing the nozzle tips fixed to the cooling nozzle header.
[0050] Hereafter, the material for which aspects of the present invention are applied will be described. There is no particular limitation on the material for which the manufacturing method according to aspects of the present invention is applied, and aspects of the present invention may be used for manufacturing any conventionally known water-atomized amorphous soft magnetic material.
[0051] Aspects of the present invention are very advantageously suitable when used to manufacture soft magnetic materials containing mainly Fe, Co, and Ni by water atomization. In particular, in the case where the total concentration (the total content of ferrous constituents) is more than 82.5 at %, the effects according to aspects of the present invention is markedly exerted, since there is a significant increase in saturated magnetic flux density (Bs) when an amorphous material fraction after atomization is more than 90% and a particle diameter (average particle diameter) is 5 m or more. In addition, aspects of the present invention have an advantageous effect that it is possible to stably obtain amorphous powder having a large particle diameter by applying aspects of the present invention to materials having chemical compositions out of the range described above more easily than by using conventional methods. Here, it is preferable that the particle diameter of the above-described powder having a large particle diameter be 100 m or less, because the upper limit of the particle diameter with which it is possible to sufficiently exert the effect described above is 100 m. In addition, the particle diameter is determined by using the method described in EXAMPLES.
EXAMPLES
[0052] The experiments described below were conducted by using the apparatuses illustrated in
[0053] After soft magnetic iron powder was collected by a hopper, dried, and classified, the iron powder was subjected to X-ray diffractometry to determine halo peaks from amorphous materials (non-crystalline materials) and diffraction peaks from crystals. Then, amorphous material fraction was calculated by using a WPPD method. Here, in the examples of the present invention and the comparative examples, the particle diameter of the soft magnetic iron powder, whose amorphous material fraction was calculated, was +63 m/75 m, and the particle diameter was classified and determined by using a sieve method. The average particle diameter of the obtained Fe-based powder (soft magnetic iron powder) was determined by, after removing contaminants which were different from the soft magnetic iron powder, using a laser diffraction/scattering-type particle size analyzer, and amorphous material fraction was calculated by performing X-ray diffractometry (by using a WPPD method).
[0054] In the examples of the present invention, soft magnetic materials having the following chemical compositions were prepared. Seven Fe-based soft magnetic materials having chemical compositions represented by, in terms of atomic percent (at %), Fe.sub.76Si.sub.9B.sub.10P.sub.5, Fe.sub.78Si.sub.9B.sub.9P.sub.4, Fe.sub.80Si.sub.8B.sub.8P.sub.4, Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2, and Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2 for Fe-based soft magnetic materials, Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1.2 for an FeCo-based soft magnetic material containing Fe and Co in a total amount of 84.8%, and Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 for an Fe-based soft magnetic material containing Fe, Co, and Ni in a total amount of 86.0%, were used. Regarding the contents, there may have been an error of about 0.3 at % or some impurities may have been contained when the raw materials were prepared, and there may have been a slight change in chemical composition due to, for example, oxidation during melting or atomization.
[0055] In example 1 of the present invention, chemical composition represented by Fe.sub.76Si.sub.9B.sub.10P.sub.5 was used, and a diameter of the molten metal-injecting nozzle of 1.9 mm was selected, which resulted in a mass ratio (Qaq/Qm) of 51.
[0056] In examples 2 and 3 of the present invention, chemical compositions represented by Fe.sub.76Si.sub.9B.sub.10P.sub.5, Fe.sub.78Si.sub.9B.sub.9P.sub.4, and Fe.sub.80Si.sub.8B.sub.8P.sub.4 were used, and the diameter of the molten metal-injecting nozzle was selected so that the mass ratio (Qaq/Qm) was 50 or more (51 to 55) in both the examples 2 and 3. In example 2, the ejection pressure of the cooling water was 25 MPa. In example 3, the temperature of the cooling water was 19 C. (1 C.)
[0057] In example 4 of the present invention, chemical compositions represented by Fe.sub.78Si.sub.9B.sub.10P.sub.5, Fe.sub.78Si.sub.9B.sub.9P.sub.4, Fe.sub.80Si.sub.8B.sub.8P.sub.4, Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2, Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2, Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1, and Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 were used, the diameter of molten metal-injecting nozzle was selected so that the mass ratio (Qaq/Qm) was 50 or more (50 to 57), the ejection pressure of the cooling water was 25 MPa or more, and the water temperature was 19 C. (1 C.)
[0058] In example 5 of the present invention, chemical compositions represented by Fe.sub.76Si.sub.9B.sub.10P.sub.5, Fe.sub.78Si.sub.9B.sub.9P.sub.4, Fe.sub.80Si.sub.8B.sub.8P.sub.4, Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2, Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2 Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1, and Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 were used, a diameter of the molten metal-injecting nozzle of 0.5 mm to 0.3 mm was selected, nitrogen gas was injected into the tundish to apply pressure to the molten metal so that the mass ratio (Qaq/Qm) was 50 or more (53 to 57), the ejection pressure of the cooling water was 25 MPa or more, and the water temperature was 19 C. (1 C.)
[0059] In the comparative example, chemical compositions represented by Fe.sub.76Si.sub.9B.sub.10P.sub.5, Fe.sub.78Si.sub.9B.sub.9P.sub.4, Fe.sub.80Si.sub.8B.sub.8P.sub.4, Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2, Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2, Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1, and Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 were used, the diameter of the molten metal-injecting nozzle was selected so that the mass ratio (Qaq/Qm) was 30 to 35, the ejection pressure was 10 MPa, and the water temperature was 32 C.
[0060] Among the results of the examples and the comparative examples, it was possible to achieve an amorphous material fraction of 98% or more, which was much larger than 90%, in the case of the examples which were within the range of the present invention. In the case of the comparative example, the amorphous material fraction was less than 90% due to an insufficient mass ratio (Qaq/Qm). From these results, it is clarified that it is possible to increase amorphous material fraction by, for example, controlling the mass ratio (Qaq/Qm) according to aspects of the present invention.
TABLE-US-00001 TABLE 1 Mass Pump Water Pressure Ferrous Example/ Ratio Ejection Tem- Applied to Nozzle Constituent Amorphous Judgement Comparative (Qaq/ Pressure perature Molten Metal Diameter [Fe + Ni + Co] Material 90% or More: Example Qm) (MPa) ( C.) Tundish (MPa) (mm) Chemical Composition (at %) (at %) Fraction (%) Less than 90%: X Example 1 51 10 32 0 1.9 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 99 Example 2 51-55 25 32 0 1.9 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 100 1.7 2Fe.sub.78Si.sub.9B.sub.9P.sub.4 78.0 99 1.6 3Fe.sub.80Si.sub.8B.sub.8P.sub.4 80.0 99 Example 3 51-55 10 19 0 1.9 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 100 1.7 2Fe.sub.78Si.sub.9B.sub.9P.sub.4 78.0 100 1.6 3Fe.sub.80Si.sub.8B.sub.8P.sub.4 80.0 99 Example 4 50-57 25 19 0 1.9 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 100 1.7 2Fe.sub.78Si.sub.9B.sub.9P.sub.4 78.0 100 1.6 3Fe.sub.80Si.sub.8B.sub.8P.sub.4 80.0 100 1.5 4Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2 82.8 100 1.5 5Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2 84.8 99 1.5 6Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1.2 84.8 99 1.5 7Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 86.0 98 Example 5 53-57 25 19 0.05~0.2 1.5 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 100 1.4 2Fe.sub.78Si.sub.9B.sub.9P.sub.4 78.0 100 1.4 3Fe.sub.80Si.sub.8B.sub.8P.sub.4 80.0 100 1.4 4Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2 82.8 100 1.3 5Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2 84.8 10 1.3 6Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1.2 84.8 99 1.3 7Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 86.0 98 Comparative 30-35 10 32 0 2.6 1Fe.sub.76Si.sub.9B.sub.10P.sub.5 76.0 70 X Example 2.5 2Fe.sub.78Si.sub.9B.sub.9P.sub.4 78.0 59 X 2.3 3Fe.sub.80Si.sub.8B.sub.8P.sub.4 80.0 43 X 2.2 4Fe.sub.82.8B.sub.11P.sub.5Cu.sub.1.2 82.8 38 X 2.2 5Fe.sub.84.8Si.sub.4B.sub.10Cu.sub.1.2 84.8 35 X 2.2 6Fe.sub.69.8Co.sub.15B.sub.10P.sub.4Cu.sub.1.2 84.8 33 X 2.2 7Fe.sub.69.8Ni.sub.1.2Co.sub.15B.sub.9.4P.sub.3.4Cu.sub.1.2 86.0 33 X
LIST OF REFERENCE SIGNS
[0061] 2 tundish [0062] 3 molten metal [0063] 4 molten metal-injecting nozzle [0064] 5 nozzle header [0065] 6 cooling nozzle [0066] 8 metal powder [0067] 14 atomizing apparatus [0068] 15 cooling-water tank [0069] 16 cooling water-temperature controller [0070] 17 high-pressure pump for atomizing cooling water [0071] 18 pipework for atomizing cooling water [0072] 20 cooling water [0073] 21 teeming nozzle bore diameter [0074] 22 tundish lid [0075] 23 inert gas-injecting port [0076] 24 pressure gauge [0077] 25 relief valve