US20160296906A1 - Ferromagnetic-particle manufacturing apparatus - Google Patents

Ferromagnetic-particle manufacturing apparatus Download PDF

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Publication number
US20160296906A1
US20160296906A1 US14/915,941 US201414915941A US2016296906A1 US 20160296906 A1 US20160296906 A1 US 20160296906A1 US 201414915941 A US201414915941 A US 201414915941A US 2016296906 A1 US2016296906 A1 US 2016296906A1
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pump
ferromagnetic
pipe
flowrate
manufacturing apparatus
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Kotaro Hirayama
Shota TANOUE
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Dai Ichi High Frequency Co Ltd
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Dai Ichi High Frequency Co Ltd
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Assigned to DAI-ICHI HIGH FREQUENCY CO., LTD. reassignment DAI-ICHI HIGH FREQUENCY CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HIRAYAMA, KOTARO, TANOUE, SHOTA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/06Solidifying liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/0018Mixed oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide [Fe3O4]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/04Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/40Nickelates
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00Heating by electric, magnetic or electromagnetic fields
    • H05B6/02Induction heating
    • H05B6/10Induction heating apparatus, other than furnaces, for specific applications
    • H05B6/105Induction heating apparatus, other than furnaces, for specific applications using a susceptor
    • H05B6/108Induction heating apparatus, other than furnaces, for specific applications using a susceptor for heating a fluid
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00Heating by electric, magnetic or electromagnetic fields
    • H05B6/64Heating using microwaves
    • H05B6/80Apparatus for specific applications
    • H05B6/806Apparatus for specific applications for laboratory use
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871Heating or cooling of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873Materials to be treated
    • B01J2219/0877Liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1209Features relating to the reactor or vessel
    • B01J2219/1212Arrangements of the reactor or the reactors
    • B01J2219/1215Single reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1209Features relating to the reactor or vessel
    • B01J2219/1221Features relating to the reactor or vessel the reactor per se
    • B01J2219/1242Materials of construction
    • B01J2219/1245Parts of the reactor being microwave absorbing, dielectric
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F2009/245Reduction reaction in an Ionic Liquid [IL]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00Metallic composition of the powder or its coating
    • B22F2301/15Nickel or cobalt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00Metallic composition of the powder or its coating
    • B22F2301/35Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C2202/00Physical properties
    • C22C2202/02Magnetic
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2214/00Aspects relating to resistive heating, induction heating and heating using microwaves, covered by groups H05B3/00, H05B6/00
    • H05B2214/04Heating means manufactured by using nanotechnology

Definitions

  • the present invention relates to a ferromagnetic-particle manufacturing apparatus.
  • ferromagnetic particles are recently used as active pharmaceutical ingredients for a magnetic resonance imaging method (MRI), a drug delivery system (DDS), a local hyperthermia treatment and so on.
  • JP2006-28032A discloses a method of generating magnetite particles, which are one type of such ferromagnetic particles, by using a coprecipitation reaction. Specifically in this method, a predetermined amount of ferrous chloride (FeCl 2 ) solution and a predetermined amount of ferric chloride (FeCl 3 ) solution are put into a reaction container. While the solutions are heated and stirred in the reaction container, sodium hydroxide (NaOH) solution is added thereto. Thus, a coprecipitation reaction between ferrous ions (Fe 2+ ) and ferric ions (Fe 3+ ) occurs so that magnetite (Fe 3 O 4 ) particles are generated.
  • FeCl 2 ferrous chloride
  • FeCl 3 ferric chloride
  • the object of the present invention is to provide a ferromagnetic-particle manufacturing apparatus capable of efficiently manufacturing ferromagnetic particles.
  • the present invention is a ferromagnetic-particle 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 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; wherein ferromagnetic particles are generated by reacting the reaction liquid.
  • the reaction liquid introduced from the one end of the pipe is heated by the microwave in the single mode cavity, so that the reaction of the reaction liquid is promoted and thus ferromagnetic particles are generated.
  • the thus generated ferromagnetic particles and the microwave are magnetically coupled.
  • a rate of a reflected wave relative to an incident wave of the microwave decreases, so that an impedance of the single mode cavity increases.
  • ferromagnetic particles are continuously generated in the pipe, without need for stirring the reaction liquid in a reaction container.
  • the reaction liquid is unlikely to vary in temperature and a 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.
  • the ferromagnetic-particle manufacturing apparatus further includes: an impedance measuring device configured to measure an impedance of the single mode cavity; and a pump-flowrate deciding unit configured to decide, based on a measurement result of the impedance measuring device, a pump flowrate by which the impedance of the single mode cavity becomes a predetermined value or more; wherein the pump is configured to introduce the reaction liquid at the pump flowrate decided by the pump-flowrate deciding unit.
  • an impedance measuring device configured to measure an impedance of the single mode cavity
  • a pump-flowrate deciding unit configured to decide, based on a measurement result of the impedance measuring device, a pump flowrate by which the impedance of the single mode cavity becomes a predetermined value or more
  • the pump is configured to introduce the reaction liquid at the pump flowrate decided by the pump-flowrate deciding unit.
  • 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.
  • the pump-flowrate deciding unit decides a pump flowrate by which the impedance becomes a predetermined value or more, and the reaction liquid is introduced from the one end of the pipe at the flowrate decided by the pump-flowrate deciding unit, a production efficiency of ferromagnetic particles can be maintained at a desired level or more.
  • an axial length of the pipe is 20 mm to 200 mm.
  • the present invention is a ferromagnetic-particle manufacturing apparatus includes: an induction heating coil; a radiofrequency power source electrically connected to the induction heating coil and configured to form an alternating field inside the induction heating coil; a pipe being disposed to pass through the inside of the induction heating coil, in which at least a partial area of the pipe in an axial direction thereof is formed of a dielectric material and an area, which is nearer to one end of the pipe than the area formed of a dielectric material, is formed of a conductive material; and a pump configured to introduce, from the one end of the pipe, an alkaline reaction liquid in which metal ions of a ferromagnetic metal and hydroxide ions are dissolved; wherein ferromagnetic particles are generated by reacting the reaction liquid.
  • the area of the pipe which is formed of a conductive material, is induction-heated by the alternating field inside the induction heating coil, and the reaction liquid introduced from the one end of the pipe is heated by the heat generated by the area formed of a conductive material, so that the reaction of the reaction liquid is promoted and thus ferromagnetic particles are generated.
  • the thus generated ferromagnetic particles function as a core (magnetic core) in the area of the pipe, which is formed of a dielectric material.
  • the inductance of the induction heating coil increases, so that the impedance of the induction heating coil increases.
  • ferromagnetic particles are continuously generated in the pipe, without need for stirring the reaction liquid in a reaction container.
  • the reaction liquid is unlikely to vary in temperature and/or a 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.
  • the ferromagnetic-particle manufacturing apparatus further includes: an impedance measuring device configured to measure an impedance of the induction heating coil; and a pump-flowrate deciding unit configured to decide, based on a measurement result of the impedance measuring device, a pump flowrate by which the impedance of the induction heating coil becomes a predetermined value or more; wherein the pump is configured to introduce the reaction liquid at the pump flowrate decided by the pump-flowrate deciding unit.
  • an impedance measuring device configured to measure an impedance of the induction heating coil
  • a pump-flowrate deciding unit configured to decide, based on a measurement result of the impedance measuring device, a pump flowrate by which the impedance of the induction heating coil becomes a predetermined value or more
  • the pump is configured to introduce the reaction liquid at the pump flowrate decided by the pump-flowrate deciding unit.
  • 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.
  • the pump-flowrate deciding unit decides a pump flowrate by which the impedance becomes a predetermined value or more, and the reaction liquid is introduced from the one end of the pipe at the flowrate decided by the pump-flowrate deciding unit, a production efficiency of ferromagnetic particles can be maintained at a desired level or more.
  • an axial length of the area of the pipe, which is formed of a conductive material is 20 mm to 200 mm.
  • the metal ions of the ferromagnetic metal are either or both of iron ions and nickel ions.
  • magnetite particles as ferromagnetic particles are generated from an alkaline reaction liquid, in which ferrous ions and ferric ions are dissolved, by means of the coprecipitation reaction between the ferrous ions and the ferric ions.
  • nickel ferrite particles as ferromagnetic particles are generated from an alkaline reaction liquid, in which ferric ions and nickel ions are dissolved, by means of the coprecipitation reaction between the ferric ions and the nickel ions.
  • sodium hydroxide is dissolved in the reaction liquid.
  • an internal diameter of the pipe is 0.3 mm to 5.0 mm.
  • an inner surface of the pipe is treated with a corrosion protective covering.
  • Glass and various synthetic resins such as polyethylene, polypropylene and fluorine resin, may be used as a covering material.
  • Polyolefin such as polyethylene and polypropylene is preferred, and polypropylene is particularly preferred. According to this embodiment, smoothness to a reaction liquid flowing through the pipe can be maintained all the time.
  • the pump-flowrate deciding unit or respective elements of the pump-flowrate deciding unit can be realized by a computer system.
  • a program for executing them in the computer system and a computer-readable storage medium storing the program are also the subject matters of the present invention.
  • 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.
  • FIG. 1 is a schematic structural view showing a ferromagnetic-particle manufacturing apparatus in a first embodiment of the present invention.
  • FIG. 2 is a schematic structural view showing a ferromagnetic-particle manufacturing apparatus in a second embodiment of the present invention.
  • FIG. 1 is a schematic structural view showing a ferromagnetic-particle manufacturing apparatus in a first embodiment of the present invention.
  • a ferromagnetic-particle manufacturing apparatus 10 in this embodiment includes: a single mode cavity 11 that resonates with a microwave of a predetermined wavelength; a microwave oscillator 12 electrically connected to the single mode cavity 11 and configured to introduce the microwave of a predetermined wavelength into the single mode cavity 11 ; a pipe 13 disposed to pass through the inside of the single mode cavity 11 , the pipe 13 being formed of a dielectric material; and pumps 14 a and 14 b configured to introduce, from one end of the pipe 13 , an alkaline reaction liquid in which metal ions of a ferromagnetic metal and hydroxide ions are dissolved.
  • 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.
  • 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 FIG. 1 .
  • the single mode cavity 11 is configured to resonate with a microwave having a wavelength of 120 mm.
  • 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 .
  • the pipe 13 in this embodiment is a resin pipe of a cylindrical shape.
  • 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.
  • the pipe 13 coaxially passes through the inside of the single mode cavity 11 , with an axis of the pipe 13 being oriented in parallel to the z direction of the single mode cavity 11 .
  • An inner surface of the pipe 13 is treated with a corrosion protective covering, so that smoothness to a liquid flowing through the pipe 13 is maintained all the time.
  • Glass and various synthetic resins such as polyethylene, polypropylene and fluorine resin, may be used as a covering material.
  • Polyolefin such as polyethylene and polypropylene is preferred, and polypropylene is particularly preferred.
  • a first liquid tank 31 is liquid-tightly connected to the one end of the pipe 13 via the pump 14 a associated with the first liquid tank 31
  • a second liquid tank 32 is liquid-tightly connected to the one end of the pipe 13 via the pump 14 b associated with the second liquid tank 32 .
  • the first liquid tank 31 accommodates a metal salt solution containing metal ions of a ferromagnetic metal.
  • metal ions of the ferromagnetic metal are either or both of iron ions and nickel ions.
  • an iron salt solution in which ferrous chloride (FeCl 2 ) and ferric chloride (FeCl 3 ) are dissolved in a molar ratio of 1:2, is accommodated in the first liquid tank 31 .
  • an iron salt solution in which ferrous sulfate (FeSO 4 ) and ferric sulfate (Fe 2 (SO 4 ) 3 ) are dissolved in a molar ratio of 1:1, may be accommodated in the first liquid tank 31 .
  • the second liquid tank 32 accommodates an alkaline solution containing hydroxide ions.
  • an alkaline solution in which sodium hydroxide (NaOH) is dissolved is accommodated in the second liquid tank 32 .
  • the pumps 14 a and 14 b 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 2+ ), ferric ions (Fe 3+ ) and hydroxide ions (OH ⁇ ) is 1:2:8.
  • reaction liquid a mixed liquid
  • reaction liquid a mixed liquid
  • ferrous ions Fe 2+
  • ferric ions Fe 3+
  • hydroxide ions OH ⁇
  • 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.
  • the impedance measuring device 15 is electrically connected to the coaxial cable 17 , and is configured to measure the impedance of the single mode cavity 11 through the coaxial cable 17 .
  • 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 .
  • 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.
  • 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.
  • a pump flowrate pump flowrate set value
  • Each of the pumps 14 a and 14 b 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 .
  • an alkaline reaction liquid in which ferrous ions (Fe 2+ ), ferric ions (Fe 3+ ) and hydroxide ions (OH ⁇ ) are dissolved in a molar ratio of 1:2:8, is introduced from the one end of the pipe 13 by the pumps 14 a and 14 b.
  • a microwave of a predetermined wavelength e.g., 120 mm is introduced from the microwave oscillator 12 into the single mode cavity 11 .
  • 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.).
  • a reaction temperature e.g. 40° C. to 80° C.
  • reaction of the reaction liquid is promoted and a coprecipitation reaction between the ferrous ions (Fe 2+ ) and the ferric ions (Fe 3+ ) occurs, whereby magnetite (Fe 3 O 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 .
  • the magnetite particles 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 .
  • 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.
  • the flowrate of each of the pumps 14 a and 14 b at this time is decided as the aforementioned pump flowrate set value.
  • the measurement result is stored in the pump-flowrate deciding unit 16 , and the pumps 14 a and 14 b are controlled such that the flowrate of the reaction liquid introduced into the the one end of the pipe 13 increases.
  • 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.
  • the pump-flowrate deciding unit 16 When the current measurement result is larger than the stored previous measurement result, the situation is judged as the case 1 , and the pumps 14 a and 14 b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 13 gradually increases.
  • 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 14 a and 14 b as the aforementioned pump flowrate set value.
  • 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 14 a and 14 b as the aforementioned pump flowrate set value.
  • each of the pumps 14 a and 14 b 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 .
  • 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 .
  • 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.
  • the thus generated ferromagnetic particles and the microwave are magnetically coupled.
  • 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.
  • a production efficiency of ferromagnetic particles in the pipe 13 can be easily estimated from outside.
  • ferromagnetic particles are continuously generated in the pipe 13 , without need for stirring the reaction liquid in the reaction container.
  • 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.
  • GMP global multi-dimensional
  • 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.
  • 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.
  • FIG. 2 is a schematic structural view showing a ferromagnetic-particle manufacturing apparatus in a second embodiment of the present invention.
  • a ferromagnetic-particle manufacturing apparatus 20 in the second embodiment includes: an induction heating coil 21 ; a radiofrequency power source 22 electrically connected to the induction heating coil 21 and configured to form an alternating field inside the induction heating coil 21 ; and a pipe 23 disposed to pass through the inside of the induction heating coil 21 .
  • At least a partial area 23 a of the pipe 23 in an axial direction thereof is formed of a dielectric material.
  • An area 23 b which is nearer to one end of the pipe 2 than the area 23 a formed of a dielectric material, is formed of a conductive material.
  • the induction heating coil 21 is a solenoid coil having a cylindrical shape.
  • a diameter of the induction heating coil 21 is 20 mm, and an axial length thereof is 150 mm.
  • 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 .
  • a predetermined frequency e.g. 20 kHz
  • the pipe 23 in this embodiment is formed by coaxially connecting a resin pipe 23 a having a cylindrical shape, and a metal pipe 23 b having a cylindrical shape that has the same internal diameter as that of the resin pipe 23 a.
  • an axial length of the resin pipe 23 a is 20 mm to 200 mm
  • an axial length of the metal pipe 23 b is 20 mm to 200 mm.
  • the internal diameters of the resin pipe 23 a and the metal pipe 23 b are both 0.3 mm to 5.0 mm.
  • a material of the resin pipe 23 a is, e.g., polyvinyl chloride, while a material of the metal pipe 23 b is e.g., stainless.
  • the pipe 23 is coaxially passes through the inside of the induction heating coil 21 , with an axis of the pipe 23 being oriented in parallel to an axis of the induction heating coil 21 .
  • a first liquid tank 31 is liquid-tightly connected to the one end of the pipe 23 on the side of the metal pipe 23 b via the pump 14 a associated with the first liquid tank 31
  • a second liquid tank 32 is liquid-tightly connected to the one end of the pipe 23 on the side of the metal pipe 23 b via the pump 14 b associated with the second liquid tank 32 .
  • An inner surface of the pipe 23 is treated with a corrosion protective covering, so that smoothness to a liquid flowing through the pipe 23 is maintained all the time.
  • an impedance measuring device 15 is incorporated in the radiofrequency power source 22 , and is configured to measure an impedance of the induction heating coil 21 .
  • the commercially available radiofrequency power source 22 incorporates the impedance measuring device 15 .
  • the impedance measuring device 15 may be located outside the radiofrequency power source 22 .
  • 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 .
  • the other structure is substantially the same as that of the first embodiment shown in FIG. 1 .
  • FIG. 2 the same part as that of the first embodiment is shown by the same reference number, and detailed description thereof is omitted.
  • an alkaline reaction liquid in which ferrous ions (Fe 2+ ), ferric ions (Fe 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 23 b by the pumps 14 a and 14 b.
  • an alternating current of a predetermined frequency e.g., 20 kHz
  • a predetermined frequency e.g. 20 kHz
  • the area (metal pipe) 23 b 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 23 b formed of a conductive material.
  • a reaction temperature e.g., 40° C. to 80° C.
  • reaction of the reaction liquid is promoted and a coprecipitation reaction between the ferrous ions (Fe 2+ ) and the ferric ions (Fe 3+ ) occurs, whereby magnetite (Fe 3 O 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) 23 a formed of a dielectric material.
  • the magnetite particles When the magnetite particles are generated in the pipe 23 , the magnetite particles function as a core (magenta core) in the area (resin pipe) 23 a 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 .
  • 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.
  • the flowrate of each of the pumps 14 a and 14 b at this time is decided as the aforementioned pump flowrate set value.
  • the measurement result is stored in the pump-flowrate deciding unit 16 , and the pumps 14 a and 14 b are controlled such that the flowrate of the reaction liquid introduced into the the one end of the pipe 23 increases.
  • 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.
  • the pump-flowrate deciding unit 16 When the current measurement result is larger than the stored previous measurement result, the situation is judged as the case 1 , and the pumps 14 a and 14 b are controlled such that the flowrate of the reaction liquid introduced to the one end of the pipe 23 gradually increases.
  • 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 14 a and 14 b as the aforementioned pump flowrate set value.
  • 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 14 a and 14 b as the aforementioned pump flowrate set value.
  • each of the pumps 14 a and 14 b 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 .
  • 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 .
  • the area 23 b 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 23 b formed of a conductive material, so that the reaction of the reaction liquid is promoted and thus ferromagnetic particles are generated.
  • the thus generated ferromagnetic particles function as a core (magnetic core) in the area 23 a of the pipe 23 , which is formed of a dielectric material.
  • 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.
  • ferromagnetic particles are continuously generated in the pipe 23 , without need for stirring the reaction liquid in the reaction container.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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 .
  • 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.
  • 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 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.
  • 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.
  • 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.
  • a 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.
  • 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.

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