Ferromagnetic-particle manufacturing apparatus
10661247 ยท 2020-05-26
Assignee
Inventors
Cpc classification
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B01J2219/0204
PERFORMING OPERATIONS; TRANSPORTING
B22F2009/245
PERFORMING OPERATIONS; TRANSPORTING
C01G53/40
CHEMISTRY; METALLURGY
B01J2219/1245
PERFORMING OPERATIONS; TRANSPORTING
B01J2219/0871
PERFORMING OPERATIONS; TRANSPORTING
B22F9/24
PERFORMING OPERATIONS; TRANSPORTING
B22F9/24
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B01J19/02
PERFORMING OPERATIONS; TRANSPORTING
International classification
B01J19/12
PERFORMING OPERATIONS; TRANSPORTING
B22F1/00
PERFORMING OPERATIONS; TRANSPORTING
B01J19/02
PERFORMING OPERATIONS; TRANSPORTING
H05B6/10
ELECTRICITY
B22F9/24
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A method for manufacturing a ferromagnetic-particle includes preparing a manufacturing apparatus including a single mode cavity that resonates with a microwave of a predetermined wavelength; a microwave oscillator electrically connected to the single mode cavity and configured to introduce the microwave of a predetermined wavelength into the single mode cavity; a pipe disposed to pass linearly through an inside of the single mode cavity, the pipe being formed of a dielectric material; and a pump configured to introduce, from one end of the pipe, an alkaline reaction liquid in which metal ions of a ferromagnetic metal and hydroxide ions are dissolved; and reacting the reaction liquid in the pipe, introduced by the pump, by introducing the microwave into the single mode cavity so as to generate the ferromagnetic-particle in the pipe.
Claims
1. A method for manufacturing a ferromagnetic-particle comprising the steps of: preparing a manufacturing apparatus including: a single mode cavity that resonates with a microwave of a predetermined wavelength; a microwave oscillator electrically connected to the single mode cavity and configured to introduce the microwave of the predetermined wavelength into the single mode cavity; a pipe disposed in the single mode cavity to pass linearly through an inside of the single mode cavity, the pipe being formed of a dielectric material; and a pump configured to introduce, from one end of the pipe, an alkaline reaction liquid in which metal ions of a ferromagnetic metal and hydroxide ions are dissolved; introducing the reaction liquid having the dissolved metal ions of the ferromagnetic metal and hydroxide ions into the pipe by the pump before heating the reaction liquid; reacting the reaction liquid in the pipe, after receiving the reaction liquid introduced by the pump, by introducing the microwave into the single mode cavity; and generating the ferromagnetic-particle in the pipe based on the reaction liquid in the pipe in the absence of a stirring action of the reaction liquid in the pipe.
2. The method according to claim 1, wherein an axial length of the pipe is 20 mm to 200 mm.
3. The method according to claim 1, wherein the metal ions of the ferromagnetic metal are either or both of iron ions and nickel ions.
4. The method according to claim 1, further comprising the step of dissolving sodium hydroxide in the reaction liquid.
5. The method according to claim 1, wherein an internal diameter of the pipe is 0.3 mm to 5.0 mm.
6. The method according to claim 1, wherein the pump includes a first pump sending a metal salt solution containing metal ions and a second pump sending an alkaline solution containing hydroxide ions.
7. The method according to claim 1, wherein the manufacturing apparatus includes an impedance measuring device configured to measure an impedance of the single mode cavity, and wherein the method further comprises the step of controlling a pump-flowrate of the reaction liquid based on a measurement result of the impedance during the reacting of the reaction liquid in the pipe, such that the impedance of the single mode cavity becomes a predetermined value.
8. The method according to claim 7, wherein: when a current measurement result of the impedance is larger than a stored previous measurement result, the pump-flowrate of the reaction liquid introduced into the pipe is controlled to gradually increase, and when the current measurement result of the impedance is smaller than the stored previous measurement result, the pump-flowrate of the reaction liquid introduced into the pipe is controlled to gradually decrease.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
(2)
MODES FOR CARRYING OUT THE INVENTION
(3) Embodiments of the present invention will be described in detail herebelow with reference to the attached drawings.
(4)
(5) As shown in
(6) The single mode cavity 11 is a hollow container made of a conductive wall such as a metal, and is also referred to as cavity resonator. The single mode cavity 11 is configured to resonate with a microwave of a predetermined wavelength which is specified depending on a size, a shape and a mode of the single mode cavity 11. Namely, inside the single mode cavity 11, only the microwave of a predetermined wavelength can exist as a standing wave. To be specific, for example, the single mode cavity 11 has a parallelepiped shape having a length of 150 mm in a right and left direction (z direction), a length of 109.2 mm in an up and down direction (y direction), and a length of 54.5 mm in a direction perpendicular to a sheet plane (x direction) in
(7) The microwave oscillator 12 is electrically connected to the single mode cavity 11 through a coaxial cable 17, and is capable of introducing the microwave of a predetermined wavelength into the single mode cavity 11.
(8) The pipe 13 in this embodiment is a resin pipe of a cylindrical shape. To be specific, for example, an internal diameter of the pipe 13 is 0.3 mm to 5.0 mm, and an axial length thereof is 20 mm to 200 mm. A material of the pipe 13 is, e.g., polyvinyl chloride.
(9) As shown in
(10) In this embodiment, as shown in
(11) The first liquid tank 31 accommodates a metal salt solution containing metal ions of a ferromagnetic metal. To be specific, for example, metal ions of the ferromagnetic metal are either or both of iron ions and nickel ions. In this embodiment, an iron salt solution, in which ferrous chloride (FeCl.sub.2) and ferric chloride (FeCl.sub.3) are dissolved in a molar ratio of 1:2, is accommodated in the first liquid tank 31. Alternatively, an iron salt solution, in which ferrous sulfate (FeSO.sub.4) and ferric sulfate (Fe.sub.2(SO.sub.4).sub.3) are dissolved in a molar ratio of 1:1, may be accommodated in the first liquid tank 31.
(12) On the other hand, the second liquid tank 32 accommodates an alkaline solution containing hydroxide ions. To be specific, for example, an alkaline solution in which sodium hydroxide (NaOH) is dissolved is accommodated in the second liquid tank 32.
(13) The pumps 14a and 14b in this embodiment are configured to introduce a mixed liquid (hereinafter referred to as reaction liquid), in which the iron salt solution accommodated in the first liquid tank 31 and the alkaline solution accommodated in the second liquid tank 32 are mixed, is introduced from the one end of the pipe 13 such that a molar flowrate of ferrous ions (Fe.sup.2+), ferric ions (Fe.sup.3+) and hydroxide ions (OH.sup.) is 1:2:8.
(14) The ferromagnetic-particle manufacturing apparatus 10 in this embodiment further includes an impedance measuring device 15 that measures an impedance of the single mode cavity 11, and a pump-flowrate deciding unit 16 that decides, based on a measurement result of the impedance measuring device 15, a pump flowrate by which the impedance of the single mold cavity 11 becomes a predetermined value or more.
(15) In this embodiment, as shown in
(16) The pump-flowrate deciding unit 16 is specifically formed of, e.g., a computer system including a storage unit storing a control program or the like. The storage unit of the pump-flowrate deciding unit 16 is configured to previously store a target value of the impedance of the single mode cavity 11. As described below, the target value may be decided based on, e.g., a measurement result change of the impedance measuring device 15 with respect to a pump flowrate change.
(17) In addition, the pump-flowrate deciding unit 16 is configured to decide, based on a measurement result of the impedance measuring device 15, a pump flowrate (pump flowrate set value) by which the impedance of the single mode cavity 11 becomes the previously stored target value or more. Each of the pumps 14a and 14b is configured to introduce the reaction liquid from the one end of the pipe 13 at the pump flow rate (pump flowrate set value) decided by the pump-flowrate deciding unit 16.
(18) Next, an operation of the embodiment as described above is described.
(19) Firstly, an alkaline reaction liquid, in which ferrous ions (Fe.sup.2+), ferric ions (Fe.sup.3+) and hydroxide ions (OFF) are dissolved in a molar ratio of 1:2:8, is introduced from the one end of the pipe 13 by the pumps 14a and 14b. In addition, a microwave of a predetermined wavelength (e.g., 120 mm) is introduced from the microwave oscillator 12 into the single mode cavity 11.
(20) The reaction liquid flowing through the pipe 13 is heated by the microwave introduced into the single mode cavity 11 up to a reaction temperature (e.g., 40 C. to 80 C.). Thus, reaction of the reaction liquid is promoted and a coprecipitation reaction between the ferrous ions (Fe.sup.2+) and the ferric ions (Fe.sup.3+) occurs, whereby magnetite (Fe.sub.3O.sub.4) particles are generated. The thus generated magnetite particles are moved by a pressure of the reaction liquid flowing through the pipe 13 so as to be taken out from the other end of the pipe 13.
(21) When the magnetite particles are generated in the pipe 13, the magnetite particles and the microwave are magnetically coupled. Thus, a rate of a reflected wave relative to an incident wave of the microwave decreases, so that an impedance of the single mode cavity 11 increases. The impedance of the single mode cavity 11 is measured by the impedance measuring device 15.
(22) The pump-flowrate deciding unit 16 reads out a measurement result from the impedance measuring device 15, and compares the measurement result with the previously stored target value.
(23) When the measurement result is equal to or larger than the target value, the flowrate of each of the pumps 14a and 14b at this time is decided as the aforementioned pump flowrate set value.
(24) On the other hand, when the measurement result is smaller than the target value, the measurement result is stored in the pump-flowrate deciding unit 16, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced into the one end of the pipe 13 increases.
(25) In principle, as the pump flowrate increases, a generation efficiency of magnetite particles also increases until the pump flowrate reaches a certain threshold value. In accordance therewith, the impedance of the single mode cavity 11 increases (case 1). However, as the pump flowrate increases after exceeding the threshold value, an unreacted reaction liquid outflows from the other end of the pipe 13, which in turn decreases the generation efficiency of magnetite particles. In accordance therewith, the impedance of the single mode cavity 11 decreases (case 2).
(26) The pump-flowrate deciding unit 16 reads out a measurement result from the impedance measuring device 15, and compares the measurement result with the stored previous measurement result.
(27) When the current measurement result is larger than the stored previous measurement result, the situation is judged as the case 1, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 13 gradually increases. During this operation, the pump-flowrate deciding unit 16 successively reads out measurement results from the impedance measuring device 15, and compares the measurement results with the previously stored target value. At a time when one of the measurement results becomes the target value or more, the pump-flowrate deciding unit 16 decides each of the flowrates of the pumps 14a and 14b as the aforementioned pump flowrate set value.
(28) On the other hand, when the current measurement result is smaller than the stored previous measurement result, the situation is judged as the case 2, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 13 gradually decreases. During this operation, the pump flow rate deciding unit 16 successively reads out measurement results from the impedance measuring device 15, and compares the measurement results with the previously stored target value. At a time when one of the measurement results becomes the target value or more, the pump-flowrate deciding unit 16 decides each of the flowrates of the pumps 14a and 14b as the aforementioned pump flowrate set value.
(29) Then, each of the pumps 14a and 14b is set such that the reaction liquid is introduced from the one end of the pipe 13 at the pump flowrate (pump flowrate set value) decided by the pump-flowrate deciding unit 16. Thus, magnetite particles are hereafter generated in the pipe 13 at a desired generation efficiency or more corresponding to the impedance target value previously stored in the pump-flowrate deciding unit 16.
(30) According to the above embodiment, the reaction liquid introduced from the one end of the pipe 13 is heated by the microwave in the single mode cavity 11, so that the reaction of the reaction liquid is promoted and thus ferromagnetic particles are generated. When ferromagnetic particles are generated in the pipe 13, the thus generated ferromagnetic particles and the microwave are magnetically coupled. Thus, a rate of a reflected wave relative to an incident wave of the microwave decreases, so that an impedance of the single mode cavity 11 increases. In this case, by measuring the impedance in the single mode cavity 11, a production efficiency of ferromagnetic particles in the pipe 13 can be easily estimated from outside.
(31) In addition, according to this embodiment, ferromagnetic particles are continuously generated in the pipe 13, without need for stirring the reaction liquid in the reaction container. Thus, the reaction liquid is unlikely to vary in temperature and the mixed condition of the reaction liquid is unlikely to be non-uniform, so that variation of the generated ferromagnetic particles in composition and dimension is small. In addition, it is easy to observe the GMP.
(32) In addition, in this embodiment, due to the application of the aforementioned principle of impedance elevation, a production efficiency of ferromagnetic particles is improved. That is to say, as the pump flowrate increases, a generation efficiency of ferromagnetic particles also increases until the pump flowrate reaches a certain threshold value. In accordance therewith, the impedance increases. However, at a pump flowrate beyond the threshold value, an unreacted reaction liquid outflows from the other end of the pipe, which in turn decreases the generation efficiency of ferromagnetic particles. In accordance therewith, the impedance decreases. Thus, in this embodiment, the pump-flowrate deciding unit 16 decides a pump flowrate by which the impedance becomes a predetermined value or more. Since the reaction liquid is introduced from the one end of the pipe 13 at the flowrate decided by the pump-flowrate deciding unit 16, a production efficiency of ferromagnetic particles can be maintained at a desired level or more.
(33) Next, a second embodiment of the present invention is described with reference to
(34)
(35) As shown in
(36) The induction heating coil 21 is a solenoid coil having a cylindrical shape. For example, a diameter of the induction heating coil 21 is 20 mm, and an axial length thereof is 150 mm.
(37) The radiofrequency power source 22 is electrically connected to the induction heating coil 21 through a radiofrequency cable 27, and is capable of supplying an alternating current of a predetermined frequency (e.g., 20 kHz) to the induction heating coil 21 so as to form an alternating field inside the induction heating coil 21.
(38) The pipe 23 in this embodiment is formed by coaxially connecting a resin pipe 23a having a cylindrical shape, and a metal pipe 23b having a cylindrical shape that has the same internal diameter as that of the resin pipe 23a. To be specific, for example, an axial length of the resin pipe 23a is 20 mm to 200 mm, and an axial length of the metal pipe 23b is 20 mm to 200 mm. The internal diameters of the resin pipe 23a and the metal pipe 23b are both 0.3 mm to 5.0 mm. A material of the resin pipe 23a is, e.g., polyvinyl chloride, while a material of the metal pipe 23b is e.g., stainless.
(39) As shown in
(40) In this embodiment, as shown in
(41) A pump-flowrate deciding unit 16 in this embodiment is configured to previously store a target value (predetermined value) of the impedance of the induction heating coil 21.
(42) The other structure is substantially the same as that of the first embodiment shown in
(43) Next, an operation of the embodiment as described above is described.
(44) Firstly, an alkaline reaction liquid, in which ferrous ions (Fe.sup.2+), ferric ions (Fe.sup.3+) and hydroxide ions (OH) are dissolved in a molar ratio of 1:2:8, is introduced from the one end of the pipe 23 on the side of the metal pipe 23b by the pumps 14a and 14b. In addition, an alternating current of a predetermined frequency (e.g., 20 kHz) is supplied from the radiofrequency power source 22 to the induction heating coil 21, so that an alternating field is formed inside the induction heating coil 21.
(45) The area (metal pipe) 23b of the pipe 23, which is formed of a conductive material, is induction-heated by the alternating field formed inside the induction heating coil 21 so as to generate heat, whereby a reaction liquid flowing through the pipe 23 is heated up to a reaction temperature (e.g., 40 C. to 80 C.) by the heat generated by the area 23b formed of a conductive material. Thus, reaction of the reaction liquid is promoted and a coprecipitation reaction between the ferrous ions (Fe.sup.2+) and the ferric ions (Fe.sup.3+) occurs, whereby magnetite (Fe.sub.3O.sub.4) particles are generated. The thus generated magnetite particles are moved by a pressure of the reaction liquid flowing through the pipe 23 so as to be taken out from the other end of the pipe 23 through the area (resin pipe) 23a formed of a dielectric material.
(46) When the magnetite particles are generated in the pipe 23, the magnetite particles function as a core (magenta core) in the area (resin pipe) 23a formed of a dielectric material. Thus, an inductance of the induction heating coil 21 increases, so that an impedance of the induction heating coil 21 increases. The impedance of the induction heating coil 21 is measured by the impedance measuring device 15.
(47) The pump-flowrate deciding unit 16 reads out a measurement result from the impedance measuring device 15, and compares the measurement result with the previously stored target value.
(48) When the measurement result is equal to or larger than the target value, the flowrate of each of the pumps 14a and 14b at this time is decided as the aforementioned pump flowrate set value.
(49) On the other hand, when the measurement result is smaller than the target value, the measurement result is stored in the pump-flowrate deciding unit 16, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced into the one end of the pipe 23 increases.
(50) In principle, as the pump flowrate increases, a generation efficiency of magnetite particles also increases until the pump flowrate reaches a certain threshold value. In accordance therewith, the impedance of the induction heating coil 21 increases (case 1). However, as the pump flowrate increases after exceeding the threshold value, an unreacted reaction liquid outflows from the other end of the pipe 23, which in turn decreases the generation efficiency of magnetite particles. In accordance therewith, the impedance of the induction heating coil 21 decreases (case 2).
(51) The pump-flowrate deciding unit 16 reads out a measurement result from the impedance measuring device 15, and compares the measurement result with the stored previous measurement result.
(52) When the current measurement result is larger than the stored previous measurement result, the situation is judged as the case 1, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 23 gradually increases. During this operation, the pump-flowrate deciding unit 16 successively reads out measurement results from the impedance measuring device 15, and compares the measurement results with the previously stored target value. At a time when one of the measurement results becomes the target value or more, the pump-flowrate deciding unit 16 decides each of the flowrates of the pumps 14a and 14b as the aforementioned pump flowrate set value.
(53) On the other hand, when the current measurement result is smaller than the stored previous measurement result, the situation is judged as the case 2, and the pumps 14a and 14b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 23 gradually decreases. During this operation, the ump flow rate deciding unit 16 successively reads out measurement results from the impedance measuring device 15, and compares the measurement results with the previously stored target value. At a time when one of the measurement results becomes the target value or more, the pump-flowrate deciding unit 16 decides each of the flowrates of the pumps 14a and 14b as the aforementioned pump flowrate set value.
(54) Then, each of the pumps 14a and 14b is set such that the reaction liquid is introduced from the one end of the pipe 23 at the pump flowrate (pump flowrate set value) decided by the pump-flowrate deciding unit 16. Thus, magnetite particles are hereafter generated in the pipe 23 at a desired generation efficiency or more corresponding to the impedance target value previously stored in the pump-flowrate deciding unit 16.
(55) According to the above embodiment, the area 23b of the pipe 23, which is formed of a conductive material, is induction-heated by the alternating field inside the induction heating coil 21, and the reaction liquid introduced from the one end of the pipe 23 is heated by the heat generated by the area 23b formed of a conductive material, so that the reaction of the reaction liquid is promoted and thus ferromagnetic particles are generated. When ferromagnetic particles are generated in the pipe 23, the thus generated ferromagnetic particles function as a core (magnetic core) in the area 23a of the pipe 23, which is formed of a dielectric material. Thus, the inductance of the induction heating coil 21 increases, so that the impedance of the induction heating coil 21 increases. In this case, by measuring the impedance of the induction heating coil 21, a production efficiency of ferromagnetic particles in the pipe 23 can be easily estimated from outside.
(56) In addition, according to this embodiment, ferromagnetic particles are continuously generated in the pipe 23, without need for stirring the reaction liquid in the reaction container. Thus, the reaction liquid is unlikely to vary in temperature and the mixed condition of the reaction liquid is unlikely to be non-uniform, so that variation of the generated ferromagnetic particles in composition and dimension is small. In addition, it is easy to observe the GMP.
(57) In addition, in this embodiment, due to the application of the aforementioned principle of impedance elevation, a production efficiency of ferromagnetic particles is improved. That is to say, as the pump flowrate increases, a generation efficiency of ferromagnetic particles also increases until the pump flowrate reaches a certain threshold value. In accordance therewith, the impedance increases. However, at a pump flowrate beyond the threshold value, an unreacted reaction liquid outflows from the other end of the pipe, which in turn decreases the generation efficiency of ferromagnetic particles. In accordance therewith, the impedance decreases. Thus, in this embodiment, the pump-flowrate deciding unit 16 decides a pump flowrate by which the impedance becomes a predetermined value or more. Since the reaction liquid is introduced from the one end of the pipe 23 at the flowrate decided by the pump-flowrate deciding unit 16, a production efficiency of ferromagnetic particles can be maintained at a desired level or more.
(58) In both the first embodiment and the second embodiment, magnetite particles as ferromagnetic particles are generated from an alkaline reaction liquid containing ferrous ions and ferric ions, by means of the coprecipitation reaction between the ferrous ions and the ferric ions. However, not limited thereto, nickel ferrite particles as ferromagnetic particles may be generated from an alkaline reaction liquid containing ferric ions and nickel ions, by means of a coprecipitation reaction between the ferric ions and the nickel ions.
(59) In addition, in both the first embodiment and the second embodiment, the pump-flowrate deciding unit 16 decides, as a pump flowrate set value, a pump flow rate by which the impedance of the single mode cavity 11 or the induction heating coil 21 becomes the previously stored target value or more, based on a measurement result of the impedance measuring device 15. However, not limited thereto, a pump flowrate by which the impedance of the single mode cavity 11 or the induction heating coil 21 becomes a maximum value may be decided as a pump flowrate set value, based on a measurement result change of the impedance measuring device 15 with respect to a pump flowrate change. Further, a pump flowrate by which the impedance of the single mode cavity 11 or the induction heating coil 21 becomes a predetermined value or more (e.g., 90% of the maximum value or more) may be decided as a pump flowrate set value, based on a measurement result change of the impedance measuring device 15 with respect to a pump flowrate change.
(60) As described above, the pump-flowrate deciding unit 16 may be constituted by a computer system, and a program for executing the pump-flowrate deciding unit 16 in the computer system and a computer-readable storage medium storing the program are also the subject matter of the present invention.
(61) Furthermore, when the pump-flowrate deciding unit 16 is realized by a program (second program) such as OS operated in the computer system, a program including various commands for controlling the program such as OS, and a storage medium storing the program are also the subject matters of the present invention.
(62) Herein, the storage medium includes one that can be recognized by itself, such as a flexible disc, and a network in which various signals are transmitted. 10 Ferromagnetic-particle manufacturing apparatus 11 Single mode cavity 12 Microwave oscillator 13 Pipe 14a Pump 14b Pump 15 Impedance measuring device 16 Pump-flowrate deciding unit 17 Coaxial cable 20 Ferromagnetic-particle manufacturing apparatus 21 Induction heating coil 22 Radiofrequency power source 23 Pipe 23a Area formed of dielectric material 23b Area formed of conductive material 24a Pump 24b Pump 25 Impedance measuring device 26 Pump-flowrate deciding unit 27 Radiofrequency cable 31 First liquid tank 32 Second liquid tank