WO2023074693A1 - 磁性線、複合磁性線、磁性線の製造方法、及び複合磁性線の製造方法 - Google Patents

磁性線、複合磁性線、磁性線の製造方法、及び複合磁性線の製造方法 Download PDF

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WO2023074693A1
WO2023074693A1 PCT/JP2022/039747 JP2022039747W WO2023074693A1 WO 2023074693 A1 WO2023074693 A1 WO 2023074693A1 JP 2022039747 W JP2022039747 W JP 2022039747W WO 2023074693 A1 WO2023074693 A1 WO 2023074693A1
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Prior art keywords
magnetic wire
phase
wire
heat
heat treatment
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PCT/JP2022/039747
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English (en)
French (fr)
Japanese (ja)
Inventor
誠 藤本
亮 丹治
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Priority to DE112022005236.8T priority Critical patent/DE112022005236T5/de
Priority to JP2023556467A priority patent/JPWO2023074693A1/ja
Priority to CN202280072410.XA priority patent/CN118176313A/zh
Priority to US18/704,880 priority patent/US20250257428A1/en
Publication of WO2023074693A1 publication Critical patent/WO2023074693A1/ja
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00—Manufacture of metal sheets, wire, rods, tubes or like semi-manufactured products by drawing
    • B21C1/02—Drawing metal wire or like flexible metallic material by drawing machines or apparatus in which the drawing action is effected by drums
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/007—Heat treatment of ferrous alloys containing Co
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/06—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
    • C21D8/1238—Flattening; Dressing; Flexing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets 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
    • H01F1/14—Magnets 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
    • H01F1/147—Alloys characterised by their composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/011—Layered products comprising a layer of metal all layers being exclusively metallic all layers being formed of iron alloys or steels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/012—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of aluminium or an aluminium alloy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
    • B32B15/015—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium the said other metal being copper or nickel or an alloy thereof
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation

Definitions

  • the present disclosure relates to a magnetic wire, a composite magnetic wire, a method of manufacturing a magnetic wire, and a method of manufacturing a composite magnetic wire.
  • the magnetic sensor includes a core made of magnetic wire and a coil wound around the core.
  • the magnetic wire undergoes rapid magnetization reversal independent of the change speed of the external magnetic field.
  • a pulse voltage is generated in the coil by electromagnetic induction accompanying this rapid magnetization reversal.
  • the magnetic sensor detects this pulse voltage as an output.
  • Patent Documents 1 to 4 disclose magnetic wires. These patent documents describe magnetic wires produced by heat-treating and twisting iron-nickel alloy wires and iron-cobalt-vanadium alloy wires.
  • Patent Documents 5 and 6 disclose a composite magnetic wire having a coating material on the outer peripheral surface of the magnetic wire. Patent Document 5 describes coating a ferromagnetic wire with a large coercive force with a ferromagnetic layer with a small coercive force and a large residual magnetization. Patent Document 6 describes coating a ferromagnetic material with a non-magnetic layer.
  • the magnetic wire of the present disclosure is A magnetic wire made of an alloy containing iron and cobalt as main components, Having a structure containing at least the ⁇ phase of the ⁇ phase and the ⁇ phase,
  • the structure has a high-angle grain boundary with a crystal orientation difference of 15 ° or more,
  • the ratio of the area of the ⁇ phase to the total area of the ⁇ phase and the ⁇ phase in the cross section of the magnetic wire is 90% or more,
  • the average crystal grain size of the ⁇ phase in the cross section is 2.5 ⁇ m or less,
  • a ratio of the length of the high-angle grain boundary to the total length of the grain boundary in the structure in the cross section is 60% or more.
  • FIG. 1 is a schematic perspective view of a magnetic wire according to an embodiment.
  • FIG. 2 is a schematic diagram showing the structure of the magnetic wire according to the embodiment.
  • FIG. 3 is a schematic diagram showing grain boundaries in the structure of the magnetic wire according to the embodiment.
  • FIG. 4 is a schematic perspective view of the composite magnetic wire according to the embodiment.
  • FIG. 5 is a schematic cross-sectional view of the composite magnetic wire according to the embodiment.
  • FIG. 6 is a schematic diagram showing twist traces in the composite magnetic wire according to the embodiment.
  • FIG. 7 shows sample No. obtained by the EBSD method.
  • 1 is a diagram showing a Phase map of No. 1.
  • FIG. 1 shows sample No. obtained by the EBSD method.
  • the performance of the magnetic sensor described above is highly dependent on the properties of the magnetic wire used in the core.
  • a magnetic wire capable of obtaining a high output is desired for miniaturization and high output of a magnetic sensor.
  • One of the purposes of the present disclosure is to provide a magnetic wire with excellent output characteristics. Another object of the present disclosure is to provide a composite magnetic wire with excellent output characteristics. Another object of the present disclosure is to provide a magnetic wire manufacturing method capable of manufacturing a magnetic wire having excellent output characteristics. Another object of the present disclosure is to provide a method for manufacturing a composite magnetic wire capable of manufacturing a composite magnetic wire with excellent output characteristics.
  • the magnetic wire of the present disclosure has excellent output characteristics.
  • the large Barkhausen phenomenon is likely to occur. That is, the higher the uniaxial anisotropy of the magnetic wire and the higher the domain wall energy, the better the output characteristics of the magnetic wire.
  • the magnetic wire is twisted. A twisted magnetic wire generates tensile residual stress along the length of the magnetic wire inside the magnetic wire.
  • the inventors obtained the following findings.
  • heat-treating a wire which is the raw material of the magnetic wire, at a specific temperature, it is made to have a specific structure in which ⁇ phase and ⁇ phase coexist.
  • a magnetic wire manufactured by twisting a wire rod having the above-mentioned specific structure can obtain a high output and has a small variation in the output.
  • the magnetic wire twisted in the state of having the above-mentioned specific structure has a new structure that has never existed before.
  • the structure of the magnetic wire satisfies specific ranges for three requirements: the area ratio of the ⁇ phase, the average crystal grain size of the ⁇ phase, and the length ratio of the high-angle grain boundaries.
  • a magnetic wire according to an embodiment of the present disclosure is A magnetic wire made of an alloy containing iron and cobalt as main components, Having a structure containing at least the ⁇ phase of the ⁇ phase and the ⁇ phase, The structure has a high-angle grain boundary with a crystal orientation difference of 15 ° or more, The ratio of the area of the ⁇ phase to the total area of the ⁇ phase and the ⁇ phase in the cross section of the magnetic wire is 90% or more, The average crystal grain size of the ⁇ phase in the cross section is 2.5 ⁇ m or less, A ratio of the length of the high-angle grain boundary to the total length of the grain boundary in the structure in the cross section is 60% or more.
  • the magnetic wire of the present disclosure has a specific structure in which the area ratio of the ⁇ phase, the average crystal grain size of the ⁇ phase, and the length ratio of the high-angle grain boundaries satisfy the above ranges.
  • the magnetic wire of the present disclosure is excellent in output characteristics by having a specific structure.
  • the ⁇ phase referred to here is a phase determined to have a body-centered cubic lattice (BCC) crystal structure by microstructural analysis by an EBSD (Electron Back Scattered Diffraction Pattern) method.
  • the ⁇ phase is, for example, at least one of a ferrite phase and a martensite phase.
  • the ⁇ phase includes a B2 ordered phase.
  • the B2 ordered phase is a phase in which Fe atoms and Co atoms are regularly arranged.
  • the ⁇ phase referred to here is a phase determined to have a face-centered cubic lattice (FCC) crystal structure by microstructural analysis by the EBSD method.
  • the ⁇ phase is, for example, the austenite phase. Methods for measuring the area ratio of the ⁇ -phase, the average crystal grain size of the ⁇ -phase, and the length ratio of the high-angle grain boundaries will be described later.
  • the magnetic wire of the present disclosure can obtain a high output, it is possible to increase the output of the magnetic sensor when the magnetic wire of the present disclosure is used for the core of the magnetic sensor described above.
  • the magnetic wire of the present disclosure can provide high output and has small variations in output. Even if the magnetic wire of the present disclosure is made smaller by reducing the diameter of the magnetic wire or shortening the length of the magnetic wire, it is easy to obtain a stable output. Therefore, it is possible to reduce the size of the magnetic sensor.
  • the alloy may have a composition containing 40% by mass or more and 70% by mass or less of cobalt, 2% by mass or more and 12% by mass or less of vanadium, and the balance being iron and unavoidable impurities.
  • the magnetic wire of (2) above is made of an alloy having the above specific composition, so that a high output can be easily obtained.
  • the alloy contains 40% to 70% by mass of cobalt, 2% to 12% by mass of vanadium, 0.1% to 1.0% by mass of silicon, and 0.05% by mass of titanium. % or more and 0.5 mass% or less, aluminum of 0.2 mass% or more and 1.0 mass% or less, and manganese of 0.2 mass% or more and 1.2 mass% or less. with the balance being iron and unavoidable impurities.
  • the magnetic wire of (3) above tends to provide higher output.
  • the structure has ⁇ 3 grain boundaries, A ratio of the length of the ⁇ 3 grain boundary to the total length of the grain boundary may be 5% or more.
  • the magnetic wire of (4) above has a specific structure in which the ratio of the length of the ⁇ 3 grain boundary satisfies the above range, so that high output and stable output can be obtained. is easy to obtain. A method for measuring the ratio of the length of the ⁇ 3 grain boundary will be described later.
  • a KAM (Kernel Average Misorientation) value of the ⁇ phase in the cross section may be 0.45° or more.
  • the magnetic wire of (5) above has a specific structure in which the KAM value of the ⁇ phase satisfies the above range, so that high output and stable output can be obtained. easy. A method for measuring the KAM value of the ⁇ -phase will be described later.
  • the magnetic wire has a diameter of 0.1 mm or more and 1.0 mm or less,
  • the magnetic wire may have a length of 25 mm or less.
  • the magnetic wire of the present disclosure provides a high output and a small variation in output. Therefore, even if the diameter of the magnetic wire is reduced or the length of the magnetic wire is shortened, a stable output can be easily obtained.
  • the magnetic wire of (6) above tends to ensure sufficient output characteristics even if the diameter or length is small. When the magnetic wire of (6) above is used for the core of a magnetic sensor, the size of the magnetic sensor can be reduced.
  • a composite magnetic wire according to an embodiment of the present disclosure is A composite magnetic wire comprising a core material and a coating material covering the outer peripheral surface of the core material,
  • the core material is made of the magnetic wire according to any one of (1) to (6) above,
  • a ratio of the diameter of the core material to the diameter of the composite magnetic wire is 45% or more and 95% or less.
  • the composite magnetic wire of the present disclosure has excellent output characteristics because the core material is made of the magnetic wire of the present disclosure. Since the composite magnetic wire of the present disclosure provides a high output, when the composite magnetic wire of the present disclosure is used for the core of the magnetic sensor described above, it is possible to increase the output of the magnetic sensor. In addition, the composite magnetic wire of the present disclosure can obtain high output and has small variations in output. The composite magnetic wire of the present disclosure can easily obtain a stable output even if it is miniaturized by reducing the diameter of the composite magnetic wire or shortening the length of the composite magnetic wire. Therefore, it is possible to reduce the size of the magnetic sensor.
  • the melting point of the coating material may be above 850°C.
  • the composite magnetic wire of (8) above can be subjected to the first heat treatment while the core material is covered with the coating material.
  • Vickers hardness of the coating material may be 200 HV or more.
  • the composite magnetic wire of (9) above tensile residual stress is likely to be introduced into the core material by twisting. As a result, the uniaxial anisotropy of the core material tends to increase, and the output characteristics of the core material tend to improve.
  • the composite magnetic wire of (9) above is likely to provide a higher output.
  • An angle of the twist mark with respect to the axis of the composite magnetic wire may be 4° or more and 60° or less.
  • a composite magnetic wire with twist marks easily maintains the tensile residual stress introduced into the core material by the twisting process. Furthermore, when the angle of the twist marks is within the above range, the tensile residual stress along the entire length of the core material tends to be introduced uniformly. As a result, the output characteristics of the core material are likely to be improved.
  • the composite magnetic wire of (10) above is likely to provide a higher output.
  • a method for manufacturing a magnetic wire a step of drawing a material made of an alloy containing iron and cobalt as main components to obtain a drawn wire; a step of subjecting the wire to a first heat treatment to obtain a first heat-treated material; A step of twisting the first heat-treated material, In the first heat treatment, the alloy structure of the first heat treated material contains an ⁇ phase and a ⁇ phase, and the ⁇ The conditions are such that the area ratio of the phase is 90% or more.
  • the magnetic wire production method of the present disclosure can produce a magnetic wire with excellent output characteristics.
  • the reason for this is that the first heat treatment controls the structure of the first heat-treated material so that it has a specific structure in which ⁇ phase and ⁇ phase coexist. By twisting the first heat-treated material having the specific structure, a magnetic wire with high output characteristics can be obtained.
  • the step of twisting may be performed under conditions such that the amount of strain on the surface of the first heat-treated material subjected to the twisting is 1.0 or more and 4.5 or less.
  • a magnetic wire with high output characteristics can be stably manufactured.
  • the magnetic wire manufacturing method of (11) or (12) above comprises: After the step of twisting, the step of subjecting the first heat-treated material after the twisting to a second heat treatment, or simultaneously with the step of performing the twisting, the first heat-treated material being twisted. A step of performing a second heat treatment may be provided. In the second heat treatment, the first heat-treated material after the twisting process or the first heat-treated material during the twisting process may be heat-treated at a temperature of 150° C. or more and 400° C. or less.
  • the output characteristics of the magnetic wire can be enhanced.
  • the drawn wire material may be heat-treated at a temperature higher than 750°C and not higher than 850°C.
  • the step of obtaining the drawn wire material may include a step of drawing the material with a workability of 10% or more.
  • a method for manufacturing a composite magnetic wire a step of obtaining a coated wire by coating the outer peripheral surface of a core material made of an alloy containing iron and cobalt as main components with a coating material; a step of drawing the coated wire to obtain a drawn wire; a step of subjecting the drawn wire material to a first heat treatment to obtain a first heat treated material; A step of twisting the first heat-treated material, In the first heat treatment, the structure of the alloy of the core material in the first heat-treated material includes an ⁇ phase and a ⁇ phase, and the ⁇ The conditions are such that the area ratio of the phase is 90% or more.
  • the method for producing a composite magnetic wire of the present disclosure can produce a composite magnetic wire with excellent output characteristics.
  • the reason for this is that the first heat treatment controls the structure of the core material in the first heat-treated material so that it becomes a specific structure in which the ⁇ phase and the ⁇ phase coexist.
  • a composite magnetic wire with high output characteristics can be obtained by twisting the first heat-treated material.
  • twisting is applied while the core material is covered with the coating material.
  • the core material is pulled by the covering material in the vicinity of the outer peripheral surface of the core material, and the core material is elongated along the length of the core material.
  • the twisting introduces a tensile residual stress into the core along the length of the core.
  • the tensile residual stress increases and the uniaxial anisotropy of the core material increases. Since the uniaxial anisotropy of the core material is increased, the output characteristics of the core material are improved.
  • the step of twisting may be performed under conditions such that the twisted surface of the first heat-treated material has a strain amount of 0.8 or more and 3.0 or less.
  • the output characteristics of the composite magnetic wire can be enhanced.
  • the drawn wire material may be heat-treated at a temperature higher than 750°C and not higher than 850°C.
  • the step of obtaining the drawn wire material may include a step of drawing the core material of the covered wire material at a workability of 10% or more.
  • FIG. 1 A magnetic wire 1 according to an embodiment will be described with reference to FIGS. 1 to 3.
  • FIG. The magnetic wire 1 generates a large Barkhausen jump phenomenon when an external magnetic field is applied.
  • the magnetic wire 1 is made of an alloy containing iron and cobalt as main components.
  • the magnetic wire 1 has a specific structure 10 and thus has excellent output characteristics.
  • the magnetic wire 1 of the embodiment will be described in detail below.
  • Fe iron. Co is cobalt.
  • V vanadium.
  • Si silicon.
  • Ti titanium.
  • Al aluminum.
  • Mn manganese.
  • Ni nickel.
  • Cr chromium.
  • Mo molybdenum.
  • Nb niobium.
  • W tungsten.
  • Cu copper.
  • the elemental content is the proportion of the element contained in the alloy expressed in mass percent. The entire alloy is 100% by weight.
  • composition The composition of the alloy forming the magnetic wire 1 contains Fe and Co as main components. "Containing Fe and Co as main components” means containing 75% by mass or more of Fe and Co in total.
  • the magnetic wire 1 can obtain good output characteristics by twisting.
  • the melting point of the alloy forming the magnetic wire 1 is, for example, about 1300.degree.
  • the composition of the magnetic wire 1 may contain Fe and Co in a total amount of 80 mass % or more, further 85 mass % or more.
  • the composition of the magnetic wire 1 may contain additional elements other than Fe and Co.
  • a specific example of the composition is a composition containing 40% by mass or more and 70% by mass or less of Co, 2% by mass or more and 12% by mass or less of V, and the balance being Fe and unavoidable impurities.
  • a magnetic wire 1 made of an alloy having such a composition can easily obtain a high output. Output characteristics improve because the Co content is 40% by mass or more and 70% by mass or less.
  • the V content is 2% by mass or more, output characteristics are improved, and twisting can be easily performed in the manufacturing process. Even if the content of V exceeds 12% by mass, no further effect is obtained, so the upper limit of the V content is 12% by mass.
  • the Co content may be 42% by mass or more and 63% by mass or less, further 45% by mass or more and 55% by mass or less, or 48% by mass or more and 53% by mass or less.
  • the V content may be 5% by mass or more and 12% by mass or less, further 7% by mass or more and 11.5% by mass or less, or 8.5% by mass or more and 11% by mass or less.
  • the composition of the magnetic wire 1 may be a composition containing, in addition to Co and V, one or more elements selected from the group consisting of Si, Ti, Al, and Mn, and the balance being Fe and unavoidable impurities. . These elements have the effect of improving the output characteristics of the magnetic wire 1 .
  • the content of Si is more than 0% by mass and 1.0% by mass or less.
  • the content of Ti is more than 0% by mass and 0.5% by mass or less.
  • the content of Al is more than 0% by mass and 1.0% by mass or less.
  • the content of Mn is more than 0% by mass and 1.2% by mass or less.
  • the Si content may be 0.1% by mass or more, and may be 0.15% by mass or more in order to obtain the above effects.
  • the content of Ti may be 0.05% by mass or more, and may be 0.08% by mass or more to obtain the above effect.
  • the Al content may be 0.2% by mass or more, and may be 0.3% by mass or more to obtain the above effect.
  • the content of Mn may be 0.2% by mass or more, and may be 0.4% by mass or more to obtain the above effect.
  • the content of Si contained as an unavoidable impurity is less than 0.1% by mass.
  • the content of Ti contained as an unavoidable impurity is less than 0.05% by mass.
  • the content of Al contained as an unavoidable impurity is less than 0.2% by mass.
  • the content of Mn contained as an unavoidable impurity is less than 0.2% by mass.
  • the Si content may be 0.1% by mass or more and 0.7% by mass or less, and further 0.15% by mass or more and 0.5% by mass or less.
  • the Ti content may be 0.05% by mass or more and 0.4% by mass or less, and further 0.08% by mass or more and 0.3% by mass or less.
  • the Al content may be 0.2 mass % or more and 0.9 mass % or less, and further 0.3 mass % or more and 0.8 mass % or less.
  • the content of Mn may be 0.2 mass % or more and 1.1 mass % or less, and further 0.3 mass % or more and 1.0 mass % or less.
  • the composition of the magnetic wire 1 may contain one or more elements selected from the group consisting of Ni, Cr, Mo, Nb, W, and Cu. These elements have the effect of improving the output characteristics of the magnetic wire.
  • the content of these elements is, for example, more than 0% by mass and 1.0% by mass or less, and further 0.2% by mass or more and 0.8% by mass or less.
  • the composition of the magnetic wire 1 can be determined by, for example, ICP emission spectrometry (Inductively Coupled Plasma Optical Emission Spectrometry) or EDX (Energy Dispersive X-ray Spectroscopy).
  • ICP emission spectrometry Inductively Coupled Plasma Optical Emission Spectrometry
  • EDX Electronic X-ray Spectroscopy
  • the alloy structure 10 that constitutes the magnetic wire 1 contains at least an ⁇ phase 11, as shown in FIG.
  • a structure 10 shown in FIG. 2 includes an ⁇ phase 11 and a ⁇ phase 12 .
  • FIG. 2 schematically shows the structure 10 in the cross section of the magnetic wire 1.
  • the ⁇ phase 12 is hatched for easy understanding.
  • the ⁇ phase 11 is, for example, at least one selected from ferrite phase, martensite phase, and B2 ordered phase. The reason for defining the ⁇ phase 11 in this way is that it is difficult to distinguish between the ferrite phase, the martensite phase, and the B2 ordered phase in a general structure analysis by the EBSD method.
  • the ⁇ phase 12 is, for example, an austenite phase.
  • the tissue 10 may or may not contain the ⁇ -phase 12 . That is, the structure 10 may be a structure containing substantially only the ⁇ phase 11 out of the ⁇ phase 11 and the ⁇ phase 12, or a structure in which the two phases of the ⁇ phase 11 and the ⁇ phase 12 coexist. may
  • the tissue 10 may contain unillustrated unavoidable phases other than the ⁇ phase 11 and the ⁇ phase 12 .
  • An unavoidable phase is, for example, an unavoidably produced precipitation phase.
  • the structure 10 of the magnetic wire 1 has high-angle grain boundaries 21 and ⁇ 3 grain boundaries 23, as shown in FIG.
  • the high-angle grain boundary 21 is a grain boundary having a crystal orientation difference of 15° or more among the grain boundaries 20 .
  • the ⁇ 3 grain boundary is a corresponding grain boundary with a ⁇ value of 3 crystallographically defined based on the CSL theory (Kronberg et al, Trans. Met. Soc. AIME, 1949, 185, 501).
  • Corresponding grain boundaries are those in which the deviation between the crystal orientation relationship at the grain boundary and the correct corresponding orientation relationship is small.
  • the shift is indicated by a rotation angle ⁇ between the rotation matrix representing the crystal orientation relationship between crystal grains adjacent to the grain boundary and the rotation matrix representing the accurate corresponding orientation relationship.
  • ⁇ c in the above standard expression means the maximum value of the allowable deviation angle that can maintain the grain boundary structure as the corresponding grain boundary.
  • a corresponding grain boundary is defined as a grain boundary in which the deviation angle from the corresponding orientation relationship with a ⁇ value of 29 or less is ⁇ c or less.
  • the ⁇ 3 grain boundary 23 is included in the high-angle grain boundary 21 .
  • FIG. 3 also schematically shows the structure 10 in the cross section of the magnetic wire 1. As shown in FIG.
  • the high-angle grain boundaries 21 are indicated by thick lines, and the ⁇ 3 grain boundaries 23 are indicated by thick dashed lines.
  • the small-angle grain boundaries 22 are indicated by thin lines. The small-angle grain boundary 22 will be described later.
  • the area ratio of the ⁇ -phase 11, the average crystal grain size of the ⁇ -phase 11, and the length ratio of the high-angle grain boundaries 21 satisfy specific ranges.
  • the magnetic wire 1 has a specific structure 10 that satisfies all of these three requirements, so that a high output can be obtained and the variation in the output is small.
  • the area ratio of the ⁇ -phase, the average crystal grain size of the ⁇ -phase, and the length ratio of the high-angle grain boundaries will be described in detail below. In the following description, "percentage of length of high-angle grain boundaries" is referred to as "percentage of high-angle grain boundaries.”
  • the area ratio of the ⁇ phase 11 shown in FIG. 2 is 90% or more.
  • the area ratio of ⁇ phase 11 is the ratio of the area of ⁇ phase 11 to the total area of ⁇ phase 11 and ⁇ phase 12 . That is, the area ratio of the ⁇ phase 11 is the ratio of the area of the ⁇ phase 11 when the sum of the area of the ⁇ phase 11 and the area of the ⁇ phase 12 is 100.
  • the area of ⁇ phase 12 includes zero. When the area of the ⁇ phase 12 is zero, the area ratio of the ⁇ phase 11 is 100%. Output characteristics of the magnetic wire 1 can be enhanced by setting the area ratio of the ⁇ phase 11 to 90% or more.
  • the area ratio of the ⁇ phase 11 may be 95% or more, and may be 98% or more.
  • the upper limit of the area ratio of the ⁇ phase 11 is, for example, 99.99%.
  • the area ratio of the ⁇ phase 11 is 90% or more and 99.99% or less, further 90% or more and 99.98% or less, 95% or more and 99.95% or less, 98% or more and 99.92% or less, 98.5% or more. It may be 99.90% or less.
  • the area ratio of the ⁇ phase 11 is obtained by the EBSD method. Specifically, the area ratio of the ⁇ -phase 11 is determined by observing the cross section of the magnetic wire 1 with a SEM (Scanning Electron Microscope) and performing crystal analysis by the EBSD method.
  • the cross section to be observed is the cross section.
  • the cross section is a cross section perpendicular to the length of the magnetic wire 1 .
  • the size of the observation field is, for example, 5.0 ⁇ m or more ⁇ 5.0 ⁇ m or more.
  • the size of the observation field is appropriately set according to the crystal grain size of the ⁇ phase 11 .
  • the magnification of the SEM is set so that 50 or more, further 100 or more crystal grains of the ⁇ -phase 11 are included in one observation field.
  • the crystal structure of the tissue 10 in the observation field is analyzed by the EBSD method. Based on the crystal structure information obtained by the EBSD method, the crystal phases such as the ⁇ phase 11 and the ⁇ phase 12 contained in the structure 10 are determined, and the area of the ⁇ phase 11 and the area of the ⁇ phase 12 are respectively measured. Discrimination of crystal phases and measurement of the area of each phase are performed using known analysis software. The area ratio of ⁇ phase 11 is calculated as ⁇ (area of ⁇ phase 11)/(area of ⁇ phase 11+area of ⁇ phase 12) ⁇ 100.
  • the ratio of the total area of the ⁇ phase 11 and the ⁇ phase 12 to the area of the structure 10 is 80% or more. In other words, the area ratio of the remainder not detected as ⁇ -phase 11 or ⁇ -phase 12 is 20% or less.
  • the remainder other than the ⁇ -phase 11 and the ⁇ -phase 12 is mainly the precipitation phase or the region where the dislocations near the grain boundaries are accumulated.
  • the ratio of the total area of the ⁇ phase 11 and the ⁇ phase 12 may be 85% or more, 90% or more, 95% or more, 98% or more, 98.5% or more, 99% or more.
  • the area of the observation field of view is regarded as the area of the tissue 10 .
  • the ratio of the total area of ⁇ phase 11 and ⁇ phase 12 can be calculated as ⁇ (area of ⁇ phase 11+area of ⁇ phase 12)/(area of observation field) ⁇ 100.
  • the average crystal grain size of the ⁇ phase 11 shown in FIG. 2 is 2.5 ⁇ m or less.
  • Output characteristics of the magnetic wire 1 can be enhanced by setting the average crystal grain size of the ⁇ phase 11 to 2.5 ⁇ m or less.
  • the average crystal grain size of the ⁇ phase 11 may be 2.3 ⁇ m or less, and further 2.1 ⁇ m or less, 1.9 ⁇ m or less, 1.6 ⁇ m or less, or 1.4 ⁇ m or less.
  • the lower limit of the average crystal grain size of the ⁇ phase 11 is, for example, 0.1 ⁇ m.
  • the average crystal grain size of the ⁇ phase 11 is 0.1 ⁇ m or more and 2.5 ⁇ m or less, further 0.2 ⁇ m or more and 2.3 ⁇ m or less, 0.3 ⁇ m or more and 2.1 ⁇ m or less, 0.4 ⁇ m or more and 1.9 ⁇ m or less, 0.6 ⁇ m 1.6 ⁇ m or more, or 0.7 ⁇ m or more and 1.4 ⁇ m or less.
  • the average crystal grain size of the ⁇ phase 11 is obtained by the EBSD method. Specifically, the average crystal grain size of the ⁇ -phase 11 is obtained by observing the cross section of the magnetic wire 1 with an SEM and performing crystal analysis by the EBSD method. The cross section to be observed is the cross section.
  • the size of the observation field is, for example, 5.0 ⁇ m or more ⁇ 5.0 ⁇ m or more.
  • the size of the observation field is appropriately set according to the crystal grain size of the ⁇ phase 11 .
  • the magnification of the SEM is set so that 50 or more, further 100 or more crystal grains of the ⁇ -phase 11 are included in one observation field.
  • the crystal orientation of the tissue 10 in the observation field is analyzed by the EBSD method.
  • a grain boundary is defined as a crystal orientation difference of 15° or more between adjacent crystal grains.
  • the grain size of all ⁇ -phases 11 contained in the structure 10 is measured.
  • the crystal grain size is measured using known analysis software.
  • the grain size of each ⁇ phase 11 is the diameter of a circle having an area equal to the area of each ⁇ phase 11 .
  • the average crystal grain size of the ⁇ phase 11 is the area-weighted average diameter of all crystal grains of the ⁇ phase 11 measured.
  • the proportion of high-angle grain boundaries 21 shown in FIG. 3 is 60% or more.
  • the ratio of the high-angle grain boundaries 21 is the ratio of the length of the high-angle grain boundaries 21 to the total length of the grain boundaries 20 in the structure 10 . That is, the ratio of the high-angle grain boundaries 21 is the ratio of the length of the high-angle grain boundaries 21 when the total length of the grain boundaries 20 is 100.
  • Output characteristics of the magnetic wire 1 can be further enhanced by setting the ratio of the high-angle grain boundaries 21 to 60% or more. From the viewpoint of improving output characteristics, the proportion of high-angle grain boundaries 21 may be 65% or more, further 70% or more, or 75% or more.
  • the upper limit of the ratio of the high-angle grain boundaries 21 is, for example, 95%.
  • the proportion of the high-angle grain boundaries 21 may be 60% or more and 95% or less, further 65% or more and 90% or less, 70% or more and 88% or less, or 75% or more and 85% or less.
  • the total length of the crystal grain boundary 20 is obtained when the crystal grain boundary 20 is divided into two: a high-angle grain boundary 21 with a crystal orientation difference of 15° or more, and a low-angle grain boundary 22 with a crystal orientation difference of 2° or more and less than 15°. , is the total length of the length of the high-angle grain boundary 21 and the length of the low-angle grain boundary 22 .
  • a grain boundary having a crystal orientation difference of less than 2° is not included in the length of the grain boundary 20 .
  • the ratio of high-angle grain boundaries 21 is obtained by the EBSD method. Specifically, the ratio of the high-angle grain boundaries 21 is determined by observing the cross section of the magnetic wire 1 with an SEM and analyzing the crystal using the EBSD method.
  • the cross section to be observed is the cross section.
  • the size of the observation field is, for example, 5.0 ⁇ m or more ⁇ 5.0 ⁇ m or more.
  • the size of the observation field is appropriately set according to the crystal grain size of the ⁇ phase 11 .
  • the magnification of the SEM is set so that 50 or more, further 100 or more crystal grains of the ⁇ -phase 11 are included in one observation field.
  • the crystal orientation of the tissue 10 in the observation field is analyzed by the EBSD method.
  • All grain boundaries 20 in the structure 10 are divided into high-angle grain boundaries 21 and low-angle grain boundaries 22 based on the crystal orientation information obtained by the EBSD method. Then, the length of the high-angle grain boundary 21 and the length of the low-angle grain boundary 22 are measured. The lengths of the high-angle grain boundaries 21 and the low-angle grain boundaries 22 are measured using known analysis software. The total length of the grain boundaries 20 is defined as the sum of the length of the high-angle grain boundaries 21 and the length of the low-angle grain boundaries 22 . The proportion of high-angle grain boundaries 21 is calculated as ⁇ (length of high-angle grain boundaries 21)/(total length of grain boundaries 20) ⁇ 100.
  • the length ratio of the ⁇ 3 grain boundaries 23 may further satisfy a specific range.
  • the magnetic wire 1 has a specific structure 10 in which the ratio of the length of the ⁇ 3 grain boundary 23 satisfies a specific range, thereby obtaining a higher output and a more stable output. is easy to obtain.
  • the ratio of the length of the ⁇ 3 grain boundary 23 will be described in detail below. In the following description, "ratio of length of ⁇ 3 grain boundary" is referred to as "ratio of ⁇ 3 grain boundary”.
  • the ratio of ⁇ 3 grain boundaries 23 shown in FIG. 3 may be 5% or more.
  • the ratio of the ⁇ 3 grain boundaries 23 is the ratio of the length of the ⁇ 3 grain boundaries 23 to the total length of the grain boundaries 20 in the structure 10 .
  • Output characteristics of the magnetic wire 1 can be further enhanced by setting the ratio of the ⁇ 3 grain boundaries 23 to 5% or more.
  • the ratio of ⁇ 3 grain boundaries 23 may be 6% or more, and may be 8% or more.
  • the upper limit of the ratio of ⁇ 3 grain boundaries 23 is, for example, 25%.
  • the ratio of the ⁇ 3 grain boundaries 23 may be 5% or more and 25% or less, further 6% or more and 22% or less, or 8% or more and 20% or less.
  • the ratio of the ⁇ 3 grain boundaries 23 is obtained from the cross section of the magnetic wire 1 by the EBSD method in the same manner as the ratio of the high-angle grain boundaries described above. Based on the crystal orientation information obtained by the EBSD method, only the ⁇ 3 grain boundary 23 is separated from all grain boundaries 20 in the structure 10 in the observation field, and the length of the ⁇ 3 grain boundary 23 is measured. Separation of the ⁇ 3 grain boundary 23 and measurement of the length of the ⁇ 3 grain boundary 23 are performed using known analysis software. The ratio of ⁇ 3 grain boundaries 23 is calculated as ⁇ (length of ⁇ 3 grain boundaries 23)/(total length of grain boundaries 20) ⁇ 100.
  • the KAM value of the ⁇ phase 11 may satisfy a specific range.
  • the magnetic wire 1 has a specific structure 10 in which the KAM value of the ⁇ phase 11 satisfies a specific range, so that a higher output and a more stable output can be obtained. easy.
  • the KAM value of the ⁇ phase 11 will be described in detail below.
  • the KAM value of the ⁇ phase 11 may be 0.45° or more. Since the KAM value of the ⁇ phase 11 is 0.45° or more, the output characteristics of the magnetic wire 1 can be enhanced. From the viewpoint of improving the output characteristics, the KAM value of the ⁇ phase 11 may be 0.47° or more, further 0.48° or more, or 0.50° or more.
  • the upper limit of the KAM value of the ⁇ phase 11 is, for example, 1.0°.
  • the KAM value of the ⁇ phase is 0.45° or more and 1.0° or less, further 0.47° or more and 0.8° or less, 0.48° or more and 0.75° or less, 0.50° or more and 0.70° It can be below.
  • the KAM value of ⁇ phase 11 is obtained by the EBSD method. Specifically, the KAM value of the ⁇ -phase 11 is obtained by observing the cross section of the magnetic wire 1 with an SEM and performing crystal analysis by the EBSD method. The cross section to be observed is the cross section. The size of the observation field is, for example, 5.0 ⁇ m or more ⁇ 5.0 ⁇ m or more. The crystal orientation of the tissue 10 in the observation field is analyzed by the EBSD method. By the EBSD method, all crystal orientation differences between adjacent spots of electron beam irradiation spots arranged with a specified step size are measured. The step size is, for example, 0.05 ⁇ m intervals.
  • the KAM value of each electron beam irradiation spot is calculated by extracting and averaging measured values with a crystal misorientation of less than 5°.
  • the KAM value of the ⁇ phase 11 is defined as the average value of the KAM values of the electron beam irradiation spots determined to be the ⁇ phase 11 in the observation field.
  • the KAM value of the ⁇ phase 11 contained in the structure 10 is calculated based on the crystal orientation information obtained by the EBSD method. Calculation of the KAM value is performed using known analysis software.
  • the KAM value has a correlation with the strain accumulation amount. It is presumed that the higher the KAM value, the greater the orientation change due to strain in the crystal grain.
  • the shape of the magnetic wire 1 can be selected appropriately.
  • the magnetic wire 1 shown in FIG. 1 is a round wire.
  • the shape of the cross section of the magnetic wire 1 is circular.
  • the cross-sectional shape of the magnetic wire 1 may be non-circular.
  • a non-circular shape is, for example, a polygonal shape, a flattened shape or an elliptical shape.
  • a polygonal shape is, for example, a square or a hexagon.
  • Quadrilaterals include rectangles, squares, trapezoids, rhombuses, and the like.
  • the elliptical shape referred to here also includes an oval shape.
  • the elliptical shape is a so-called racetrack shape, and is a shape composed of two parallel straight lines and two semicircular arcs connecting the ends of the two straight lines. Two straight lines are equal in length. The lengths of the two half arcs are equal.
  • the term "flat shape” as used herein means a general shape that is flatter than a perfect circle. A flat shape also includes a rectangular shape, an elliptical shape, and the like.
  • the diameter D of the magnetic wire 1 can be selected as appropriate.
  • the diameter D of the magnetic wire 1 here is the diameter of a circle having an area equal to the cross-sectional area of the magnetic wire 1 .
  • a diameter D of the magnetic wire 1 is, for example, 0.1 mm or more and 1.0 mm or less.
  • the magnetic wire 1 having a diameter D within the above range can be suitably used for cores such as magnetic sensors.
  • the diameter D of the magnetic wire 1 may be 0.15 mm or more and 0.8 mm or less, and further 0.2 mm or more and 0.6 mm or less.
  • the cross-sectional area of the magnetic wire 1 can be appropriately selected.
  • the cross-sectional area of the magnetic wire 1 is the cross-sectional area of the magnetic wire 1 .
  • the cross-sectional area of the magnetic wire 1 is, for example, 0.007 mm 2 or more and 0.8 mm 2 or less.
  • the magnetic wire 1 having a cross-sectional area within the above range can be suitably used for cores of magnetic sensors and the like.
  • the cross-sectional area of the magnetic wire 1 may be 0.017 mm 2 or more and 0.51 mm 2 or less, and further 0.03 mm 2 or more and 0.3 mm 2 or less.
  • the length L of the magnetic wire 1 can be selected appropriately.
  • the length L of the magnetic wire 1 is the length from the first end to the second end of the magnetic wire 1 .
  • the length L of the magnetic wire 1 is, for example, 3 mm or more and 25 mm or less.
  • the magnetic wire 1 whose length L is within the above range can be suitably used for cores of magnetic sensors and the like.
  • the length L of the magnetic wire 1 may be 4 mm or more and 20 mm or less, or 5 mm or more and 15 mm or less.
  • the magnetic wire 1 of the embodiment can obtain a high output and has a small variation in output. Therefore, even if the diameter D or the length L is small, it is easy to secure sufficient output characteristics.
  • the size of the magnetic sensor can be reduced.
  • the magnetic wire 1 of the embodiment can be manufactured by the magnetic wire manufacturing method of the embodiment.
  • a method for manufacturing a magnetic wire according to an embodiment includes the following first step, second step, and third step.
  • the first step is a step of drawing a raw material to obtain a drawn wire material.
  • the second step is a step of subjecting the drawn wire material to a first heat treatment to obtain a first heat-treated material.
  • the third step is a step of twisting the first heat-treated material.
  • a drawn wire material is produced by drawing the raw material.
  • the material is an alloy containing iron and cobalt as main components.
  • the composition of the alloy constituting the material is the composition described in the section on the composition of the magnetic wire.
  • the composition of the material is the same as the composition of the magnetic wire to be manufactured.
  • the melting point of the material is higher than the temperature of the first heat treatment.
  • the melting point of the material is, for example, about 1300.degree.
  • the material is, for example, a cast material or an extruded material.
  • Cast materials include continuously cast materials and continuously cast and rolled materials.
  • the material may be a continuously cast material.
  • the continuously cast rolled material has little variation in structure and high productivity.
  • Drawing is a method of working a material into a wire rod with a hole die or a roller die.
  • the drawing process includes drawing by a roller die, drawing by a Turks head, etc., in addition to the usual drawing by passing a material through a hole of a hole die.
  • Cold drawing facilitates obtaining a drawn wire with high dimensional accuracy.
  • the raw material is processed into a wire drawing material of a predetermined shape, and the diameter of the wire drawing material is a predetermined diameter.
  • the cross-sectional shape of the drawn wire is the same as the cross-sectional shape of the magnetic wire to be manufactured.
  • the diameter of the drawn wire is the same as the diameter of the magnetic wire to be manufactured.
  • the drawing process may be performed multiple times until the diameter of the drawn wire reaches a predetermined diameter.
  • the heat treatment may be performed during the drawing process.
  • the main purpose of this heat treatment is to soften the wire in the middle of the drawing process to improve workability.
  • This heat treatment is called intermediate heat treatment.
  • the temperature of the intermediate heat treatment is, for example, 750° C. or higher and 1100° C.
  • the temperature of the intermediate heat treatment may be 780° C. or higher and 900° C. or lower, and further 780° C. or higher and 850° C. or lower.
  • the time for the intermediate heat treatment is, for example, 10 minutes or more and 720 minutes or less.
  • the intermediate heat treatment may be performed in a hydrogen atmosphere. After performing the intermediate heat treatment, the wire is cooled.
  • the cooling rate after the intermediate heat treatment is, for example, 1° C./second or more.
  • the cooling rate may also be 5° C./s or higher, especially 10° C./s or higher. The faster the cooling rate, the easier it is to improve the workability of the wire. If the cooling rate is too slow, ordered transformation will occur, resulting in poor workability of the wire.
  • the first step may include a step of drawing the material at a processing rate of 10% or more when processing the material into a wire drawing material.
  • this workability is the workability from the final intermediate heat treatment to the final drawing process.
  • the degree of working when the above intermediate heat treatment is performed is the difference between the cross-sectional area of the wire rod at the stage where the last intermediate heat treatment is performed and the cross-sectional area of the drawn wire after the final drawing process. It is the ratio divided by the cross-sectional area of the wire at the stage of For example, consider the case where five drawing operations are performed. Suppose that intermediate heat treatments are performed between the second drawing process and the third drawing process, and between the third drawing process and the fourth drawing process. It is assumed that the intermediate heat treatment is not performed after the fourth drawing.
  • the intermediate heat treatment performed between the third drawing and the fourth drawing is the final intermediate heat treatment.
  • the drawing is performed so that the degree of processing from the diameter of the wire after the third drawing to the diameter of the wire after the fifth drawing is 10% or more.
  • the workability is the same as the total workability from the start to the end of drawing.
  • the total degree of drawing is a ratio obtained by dividing the difference between the cross-sectional area of the raw material before drawing and the cross-sectional area of the drawn wire after final drawing by the cross-sectional area of the raw material before drawing.
  • the workability is 10% or more, it is easy to control the structure of the drawn wire material so that it has a predetermined structure.
  • the structure of the finally manufactured magnetic wire tends to be the structure described in the section on the structure of the magnetic wire.
  • the degree of working may be 30% or more, and may be 40% or more.
  • the upper limit of the workability is, for example, 99.99%, although it depends on the diameter of the raw material or the diameter of the drawn wire rod to be produced.
  • the workability may be 10% or more and 99.99% or less, further 30% or more and 99.9% or less, or 40% or more and 99.5% or less.
  • a first heat-treated material is produced by subjecting the drawn wire material to a first heat treatment. After performing the first heat treatment, the first heat treated material is cooled to room temperature. Room temperature is 20°C ⁇ 15°C.
  • the alloy structure of the first heat treated material contains an ⁇ phase and a ⁇ phase, and the ratio of the area of the ⁇ phase to the total area of the ⁇ phase and ⁇ phase in the cross section of the first heat treated material is It is carried out under conditions such that it becomes 90% or more.
  • the first heat treatment may be performed in a hydrogen atmosphere.
  • the structure of the first heat-treated material is controlled to be the specific structure in which the ⁇ phase and the ⁇ phase coexist. As a result, a magnetic wire having the structure described in the section on the structure of the magnetic wire is obtained.
  • the temperature of the first heat treatment may be set within a specific range.
  • the drawn wire may be heat-treated at a temperature of more than 750° C. and 850° C. or less. If the temperature of the first heat treatment is too low, it becomes difficult to twist the first heat treated material in the third step.
  • the temperature of the first heat treatment is low, the area ratio of the ⁇ phase becomes small, the KAM value of the ⁇ phase becomes small, and the average crystal grain size of the ⁇ phase becomes large.
  • the temperature of the first heat treatment is low, high-angle grain boundaries or ⁇ 3 grain boundaries are not sufficiently formed, and the ratio of high-angle grain boundaries or ⁇ 3 grain boundaries decreases. If the temperature of the first heat treatment is too high, the crystal grains of the prior ⁇ phase before martensite transformation become coarse. As a result, the average crystal grain size of the ⁇ -phase produced after cooling increases.
  • the optimum temperature range for the first heat treatment varies depending on the composition of the alloy. For example, in the case of a composition containing 40% by mass or more and 70% by mass or less, particularly 45% by mass or more and 55% by mass or less of Co, the temperature of the first heat treatment is 760°C or more and 840°C or less, 780°C or more and 820°C or less, and further 790°C. It may be above 810° C. or below.
  • the time for the first heat treatment is, for example, 10 minutes or more and 720 minutes or less.
  • the cooling rate after the first heat treatment is, for example, 1°C/second or more.
  • the cooling rate may also be 5° C./s or higher, especially 10° C./s or higher.
  • the faster the cooling rate the greater the area fraction of the ⁇ phase due to martensite transformation. Therefore, it is easy to obtain the above specific structure. If the cooling rate is too slow, the workability of the first heat-treated material may deteriorate due to ordered transformation. On the other hand, if the cooling rate is too slow, martensite transformation does not occur sufficiently and the area ratio of the ⁇ phase becomes small.
  • the first heat-treated material is twisted. Twisting refers to twisting with the axis of the first heat-treated material as the axis of rotation. Before twisting, the first heat-treated material should be cut to an appropriate length. By twisting the first heat-treated material, a magnetic wire with high output characteristics can be obtained. A strain-induced transformation occurs by twisting. Therefore, the ⁇ phase in the structure of the first heat treated material transforms into the ⁇ phase, and the ⁇ phase increases in the structure of the first heat treated material that has been twisted. Twisting may be done cold. After twisting, the twisted first heat-treated material is cut into a predetermined length. This predetermined length is the same as the length of the magnetic wire to be manufactured.
  • the twisting process may be performed under conditions such that the amount of strain on the surface of the first heat-treated material subjected to the twisting process is 1.0 or more and 4.5 or less.
  • the surface of the first heat-treated material here means the outer peripheral surface of the first heat-treated material.
  • a magnetic wire with high output characteristics can be stably produced by twisting so that the strain amount is 1.0 or more and 4.5 or less.
  • the strain amount may be 1.5 or more and 4.0 or less.
  • the magnetic wire 1 shown in FIG. 1 is regarded as the first heat-treated material.
  • the first heat-treated material is called "wire”.
  • the amount of strain is determined by the total number of rotations in addition to the radius and length of the wire.
  • the twisting conditions can be changed as appropriate.
  • one set may consist of a set of twisting in the clockwise direction and b turns in the counterclockwise direction, and this may be repeated in a plurality of sets.
  • the work of twisting c in the clockwise direction, d in the counterclockwise direction, and e in the clockwise direction may be set as one set, and this may be repeated in a plurality of sets.
  • the total number of rotations clockwise and the total number of rotations counterclockwise may be different.
  • the magnetic wire manufacturing method of the embodiment may include, after the third step of twisting, a step of subjecting the twisted first heat-treated material to a second heat treatment, or performing the twisting. Simultaneously with the steps, the first heat treated material being twisted may be subjected to a second heat treatment.
  • the twisting is finished when the first heat-treated material is twisted, and the second heat treatment is performed while the first heat-treated material is still twisted. you can go
  • the twisting process is performed, for example, by rotating one of the chucks while gripping both ends of the wire with chucks.
  • Performing the second heat treatment at the same time as twisting means not only performing the second heat treatment while twisting the wire, but also in a state where twisting stress is applied to the wire even after the final twist is applied to the wire. It also includes the case where the second heat treatment is performed while the wire is gripped by the chuck.
  • the first heat treated material after twisting or the first heat treated material during twisting is heat treated at a temperature of, for example, 150°C or higher and 400°C or lower.
  • a temperature of the second heat treatment By setting the temperature of the second heat treatment within the above specific range, the non-uniformly induced strain becomes uniform, so that the output characteristics of the manufactured magnetic wire can be enhanced. If the temperature of the second heat treatment is too high, the average crystal grain size of the ⁇ -phase will increase, or the area ratio of the ⁇ -phase will decrease as the ⁇ -phase increases. As a result, the output characteristics of the magnetic wire may deteriorate.
  • the temperature of the second heat treatment may be 250° C. or higher and 375° C. or lower, and further 300° C. or higher and 350° C. or lower.
  • the time for the second heat treatment is, for example, 10 minutes or more and 720 minutes or less.
  • the magnetic wire 1 of the embodiment has a specific structure 10 and thus has excellent output characteristics.
  • the magnetic wire 1 has a structure 10 that satisfies specific ranges for the area ratio of the ⁇ phase 11, the average crystal grain size of the ⁇ phase 11, and the ratio of the high-angle grain boundaries 21, so that high output is achieved. It is obtained, and the variation of the output is small.
  • the magnetic wire 1 has a structure 10 in which at least one of the ratio of the ⁇ 3 grain boundary 23 and the KAM value of the ⁇ phase 11 satisfies a specific range, so that a higher output can be obtained. .
  • the first heat treatment is performed so as to obtain a specific structure in which the ⁇ phase and the ⁇ phase coexist, and then the first heat treated material is twisted to improve the output characteristics. can obtain a magnetic wire with a high
  • FIG. 5 shows a cross section of the composite magnetic wire 2. As shown in FIG. The cross section is a cross section perpendicular to the length of the composite magnetic wire 2 .
  • the core material 30 is made of the magnetic wire 1 of the embodiment described above.
  • the core material 30 develops a large Barkhausen jump phenomenon when an external magnetic field is applied.
  • the core material 30 is made of an alloy containing Fe and Co as main components.
  • the core material 30 has the same composition as that of the alloy forming the magnetic wire 1 described above.
  • the composition of the core material 30 is as described in the section on the composition of the magnetic wire.
  • the melting point of the core material 30 is, for example, about 1300.degree.
  • the core material 30 has the same structure as that of the alloy forming the magnetic wire 1 described above.
  • the area ratio of the ⁇ phase, the average crystal grain size of the ⁇ phase, and the ratio of high-angle grain boundaries satisfy specific ranges.
  • the core material 30 has a particular texture that meets all three of these requirements.
  • a core material 30 having a specific structure has excellent output characteristics.
  • the composite magnetic wire 2 having such a core material 30 can obtain a high output and has a small variation in the output.
  • the core material 30 may have a ratio of ⁇ 3 grain boundaries that satisfies a specific range.
  • the core material 30 may have an ⁇ -phase KAM value that satisfies a specific range.
  • the core material 30 has a structure in which at least one of the ratio of ⁇ 3 grain boundaries and the KAM value of the ⁇ phase satisfies a specific range, so that the composite magnetic wire 2 can obtain a higher output.
  • the specific ranges of the area ratio of the ⁇ phase, the average crystal grain size of the ⁇ phase, the ratio of high-angle grain boundaries, the ratio of ⁇ 3 grain boundaries, and the KAM value of the ⁇ phase are described in the section on the structure of the magnetic wire described above. That's right.
  • the covering material 40 is made of metal.
  • the metal forming the coating material 40 is, for example, iron or an iron alloy, copper or a copper alloy, aluminum or an aluminum alloy, and nickel or a nickel alloy.
  • Iron alloys are, for example, stainless steel or carbon steel.
  • Stainless steel is, for example, SUS403, SUS430, SUS304, SUS316, SUS304L, or SUS316L.
  • a copper alloy is, for example, phosphor bronze.
  • Nickel alloys are, for example, permalloy, nitinol, or nichrome.
  • Coating material 40 may be a magnetic or non-magnetic material. Metal has moderate elongation. Since the covering material 40 is made of metal, it can be easily twisted in the manufacturing process.
  • the covering material 40 is made of metal, the output characteristics of the core material 30 are likely to be improved by twisting. As a result, the composite magnetic wire 2 can easily obtain a high output.
  • the material of the coating material 40 can be specified, for example, from analysis results of the composition of the coating material 40 by the EDX method.
  • the reason why the output characteristics of the core material 30 are improved by providing the coating material 40 on the core material 30 is considered as follows.
  • the core material 30 is pulled by the coating material 40 in the vicinity of the outer peripheral surface of the core material 30, and the core material 30 is elongated along the length of the core material 30.
  • the twisting introduces a tensile residual stress into the core 30 along the length of the core 30 .
  • the uniaxial anisotropy of the core material 30 increases due to an increase in tensile residual stress. Since the uniaxial anisotropy of the core material 30 is increased, the output characteristics of the core material 30 are improved.
  • the covering material 40 is clad on the core material 30 .
  • the coating material 40 is clad with the core material 30 means that the cylindrical coating material 40 is fitted to the outer peripheral surface of the core material 30 and joined.
  • the covering material 40 may be plated on the outer peripheral surface of the core material 30 .
  • the Vickers hardness of the covering material 40 is, for example, 200HV or more. The higher the hardness of the coating material 40, the more likely it is that tensile residual stress will be introduced into the core material 30 by twisting. As a result, the output characteristics of the core material 30 are likely to be improved.
  • the Vickers hardness of the coating material 40 may be 300 HV or more, and may be 380 HV or more.
  • the upper limit of the Vickers hardness of the covering material 40 is, for example, 700HV.
  • the Vickers hardness of the covering material 40 may be 200 HV or more and 700 HV or less, further 300 HV or more and 600 HV or less, or 380 HV or more and 480 HV or less.
  • the Vickers hardness of the covering material 40 is determined as follows. A cross section of the composite magnetic wire 2 is taken. Specifically, after embedding the composite magnetic wire 2 in resin, the composite magnetic wire 2 is cut along a plane orthogonal to the length of the composite magnetic wire 2 . The cross section of the exposed composite magnetic wire 2 is polished. The midpoint of the thickness of the covering material 40 is obtained in the cross section of the composite magnetic wire 2 . The midpoint of the thickness of the covering material 40 is the midpoint between the inner circumference and the outer circumference of the covering material 40 . As shown in FIG.
  • the midpoint of the thickness of the covering material 40 is the sum of the inner diameter and the outer diameter of the covering material 40 divided by two. located on the circumference of concentric circles with The inner diameter of the covering material 40 is equal to the diameter D1 of the core material 30, and the outer diameter of the covering material 40 is equal to the diameter D2 of the composite magnetic wire 2. That is, the diameter of this concentric circle is (D1+D2)/2.
  • a micro Vickers hardness test is performed on four points among the intermediate points of the thickness.
  • the Vickers hardness of the covering material 40 is regarded as the average value of the four measured Vickers hardnesses.
  • the four points are arranged around the central axis of the covering material 40 at regular intervals.
  • the micro Vickers hardness test is performed in accordance with JIS Z 2244:2009 "Vickers hardness test”.
  • the test force is 0.098N (0.01kgf).
  • the Vickers hardness of the core material 30 is, for example, about 400HV to about 500HV.
  • the Vickers hardness of the core material 30 is determined as follows. Find the midpoint of the radius of the core material 30 in the cross section of the composite magnetic wire 2 .
  • the midpoint of the radius of the core material 30 is the midpoint between the center of the core material 30 and a point on the outer periphery of the core material 30 .
  • the midpoint of the radius of the core material 30 is on the circumference of a concentric circle having a diameter of 1/2 of the diameter of the core material 30. Located in That is, the diameter of this concentric circle is D1/2.
  • a micro Vickers hardness test is performed on four points among the midpoints of the diameter.
  • the Vickers hardness of the core material 30 is regarded as the average value of the measured four Vickers hardnesses.
  • the four points are arranged around the central axis of the core material 30 at regular intervals.
  • the melting point of the covering material 40 is above 850° C., for example. If the melting point of the coating material 40 is higher than 850° C., the first heat treatment described later can be performed in the state where the core material 30 is coated with the coating material 40 in the manufacturing process.
  • the melting point of the covering material 40 may be 900° C. or higher, or even 950° C. or higher.
  • the melting point of the covering material 40 is obtained as follows.
  • the initial shape of the composite magnetic wire 2 is measured. For example, the diameter of the composite magnetic wire 2 is measured.
  • a cooling process is performed.
  • the melting point of the covering material 40 is the heating temperature at which the covering material 40 melts and changes its shape.
  • a specific method for measuring the melting point is as follows. After heating the composite magnetic wire 2 to a predetermined temperature, it is cooled. By comparing the shape of the composite magnetic wire 2 after cooling with the initial shape, it is confirmed whether or not the covering material 40 has melted. If the covering material 40 is not melted, the composite magnetic wire 2 is heated to a higher temperature and then cooled.
  • the heating temperature is set, for example, from 100°C to 1300°C in increments of 50°C.
  • the time for holding the composite magnetic wire 2 in a heated state is, for example, 5 minutes or longer.
  • the shape of the composite magnetic wire 2 can be appropriately selected.
  • the composite magnetic wire 2 shown in FIGS. 4 and 5 is a round wire.
  • the cross-sectional shape of the composite magnetic wire 2 is circular.
  • the cross-sectional shape of the composite magnetic wire 2 may be non-circular.
  • a non-circular shape is, for example, a polygonal shape, a flattened shape or an elliptical shape.
  • a polygonal shape is, for example, a square or a hexagon.
  • Quadrilaterals include rectangles, squares, trapezoids, rhombuses, and the like.
  • Elliptical shapes also include oblong shapes.
  • a flat shape means a flat shape in general.
  • a flat shape also includes a rectangular shape, an elliptical shape, and the like.
  • the shape of the cross section of the core material 30 shown in FIGS. 4 and 5 is circular.
  • the cross-sectional shape of the covering material 40 is cylindrical.
  • the diameter D2 of the composite magnetic wire 2 can be selected as appropriate.
  • the diameter D2 of the composite magnetic wire 2 here is the diameter of a circle having an area equal to the area of the cross section of the composite magnetic wire 2 .
  • a diameter D2 of the composite magnetic wire 2 is, for example, 0.105 mm or more and 3.0 mm or less.
  • a composite magnetic wire 2 having a diameter D2 within the above range can be suitably used for a core of a magnetic sensor or the like.
  • the diameter D2 of the composite magnetic wire 2 may be 0.11 mm or more and 2.0 mm or less, 0.12 mm or more and 1.0 mm or less, 0.15 mm or more and 0.8 mm or less, and further 0.2 mm or more and 0.6 mm or less.
  • the length L2 of the composite magnetic wire 2 can be selected appropriately.
  • the length L2 of the composite magnetic wire 2 is the length from the first end to the second end of the composite magnetic wire 2 .
  • the length L2 of the composite magnetic wire 2 is, for example, 3 mm or more and 25 mm or less.
  • a composite magnetic wire 2 having a length L2 within the above range can be suitably used for a core of a magnetic sensor or the like.
  • the length L2 of the composite magnetic wire 2 may be 4 mm or more and 20 mm or less, or 5 mm or more and 15 mm or less.
  • the composite magnetic wire 2 of the embodiment can obtain a high output and has a small variation in output. Therefore, even if the diameter D2 or the length L2 is small, it is easy to secure sufficient output characteristics.
  • the composite magnetic wire 2 having the diameter D2 and the length L2 within the above ranges is used for the core of the magnetic sensor, the size of the magnetic sensor can be reduced.
  • the ratio of the diameter D1 of the core material 30 to the diameter D2 of the composite magnetic wire 2 shown in FIG. 5 may be 45% or more and 95% or less.
  • “the ratio of the diameter of the core material to the diameter of the composite magnetic wire” is referred to as "the ratio of the core material”.
  • the diameter D1 of the core material 30 is the diameter of a circle having an area equal to the cross-sectional area of the core material 30 .
  • the ratio of the core material 30 is the ratio obtained by dividing the diameter D1 of the core material 30 by the diameter D2 of the composite magnetic wire 2 .
  • the ratio of the core material 30 is 45% or more, the area ratio of the core material 30 to the cross section of the composite magnetic wire 2 can be ensured.
  • the output characteristics of the composite magnetic wire 2 can be enhanced by ensuring the area ratio of the core material 30 to some extent.
  • the ratio of the core material 30 is set to 95% or less, the area ratio of the covering material 40 to the cross section of the composite magnetic wire 2 can be ensured.
  • tensile residual stress is likely to be introduced into the core material 30 by twisting. Since tensile residual stress is likely to be introduced into the core material 30, the uniaxial anisotropy of the core material 30 is likely to increase.
  • the ratio of the core material 30 may be 48% or more and 95% or less, 55% or more and 90% or less, or even 60% or more and 85% or less.
  • the diameter D1 of the core material 30 is, for example, 0.1 mm or more and 1.0 mm or less.
  • the composite magnetic wire 2 in which the diameter D1 of the core material 30 is within the above range is likely to provide a high output.
  • the diameter D1 of the core material 30 may be 0.15 mm or more and 0.8 mm or less, and further 0.2 mm or more and 0.6 mm or less.
  • the composite magnetic wire 2 may have twist traces 50 on the outer peripheral surface of the covering material 40, as shown in FIG. Twisting traces 50 may be present on the outer peripheral surface of the coating 40 of the composite magnetic wire 2 that has been twisted.
  • the twist marks 50 are formed by twisting the core material 30 covered with the covering material 40 in the manufacturing process.
  • the wire rod in which the outer peripheral surface of the core material is coated with the coating material may be drawn before the twisting process.
  • a plurality of traces of wire drawing are formed on the surface of the wire that has been subjected to the drawing process, that is, on the outer peripheral surface of the covering material.
  • a wire drawing trace is a thin streak-like trace extending linearly along the length of the wire.
  • Wire-drawing traces are produced by rubbing with a die or the like during the drawing process. Wire drawing traces are formed over the entire length of the wire. When the wire rod is twisted, the traces of wire drawing are deformed to form twist traces 50 .
  • the surface of the wire may be deformed and the twist mark 50 may be formed by twisting the wire.
  • the twist marks 50 are inclined with respect to the axis of the composite magnetic wire 2 as shown in FIG. Remaining in a twisted state means that the twisting process is completed while the wire is in a twisted state.
  • the twisted composite magnetic wire 2 is obtained by rotating the wire only in one direction during the twisting process.
  • the composite magnetic wire 2 in the twisted state is rotated clockwise and counterclockwise during twisting, the total number of rotations in the clockwise direction is different from the total number of rotations in the counterclockwise direction. obtained by doing
  • the angle ⁇ t of the twist marks 50 may be 4° or more and 60° or less.
  • the angle of the twist marks may be 5° or more and 55° or less, and further 20° or more and 40° or less.
  • the angle ⁇ t of the twist mark 50 can be obtained as follows.
  • the surface of the composite magnetic wire 2, that is, the outer peripheral surface of the covering material 40 is observed with an optical microscope.
  • the inclination angle of the twist mark 50 with respect to the axis of the composite magnetic wire 2 is measured.
  • the inclination angles of 20 or more twist marks 50 are measured, and the average value is taken as the angle ⁇ t of the twist marks 50 .
  • the composite magnetic wire 2 of the embodiment can be manufactured by the manufacturing method of the composite magnetic wire of the embodiment.
  • the manufacturing method of the composite magnetic wire of the embodiment includes the following first step, second step, third step and fourth step.
  • the first step is a step of obtaining a covered wire by covering the outer peripheral surface of the core material with a covering material.
  • the second step is a step of drawing the coated wire to obtain a drawn wire.
  • the third step is a step of subjecting the drawn wire material to a first heat treatment to obtain a first heat-treated material.
  • the fourth step is a step of twisting the first heat-treated material.
  • the steps proceed in the order of [coating] ⁇ [wire drawing] ⁇ [first heat treatment] ⁇ [twisting]. Each step will be described in detail below.
  • a coated wire is manufactured by coating the outer peripheral surface of the core material with a coating material.
  • the core material is made of an alloy containing iron and cobalt as main components.
  • a cast material or an extruded material can be used as the core material.
  • the covering material is made of metal.
  • the coating material can be formed on the outer peripheral surface of the core material by, for example, a clad method or a plating method.
  • the cladding method is a method of joining a coating material to the outer peripheral surface of a core material by inserting a core material into a cylindrical coating material and pulling it out.
  • the thickness of the covering material may be appropriately selected so that the ratio of the core material in the manufactured composite magnetic wire is within the above-described specific range.
  • the thickness of the covering material should be selected so that the ratio of the core material in the finally manufactured composite magnetic wire is 45% or more and 95% or less.
  • the melting point of the core material and the melting point of the covering material are higher than the temperature of the first heat treatment.
  • the melting point of the core material and the melting point of the covering material are, for example, above 850°C.
  • the melting point of the core material and the melting point of the covering material may be different or the same.
  • a drawn wire is produced by drawing the coated wire.
  • the second step is the same as the first step in the magnetic wire manufacturing method described above.
  • the second step in the manufacturing method of the composite magnetic wire is different from the first step in the manufacturing method of the magnetic wire described above in that the coated wire is drawn.
  • the drawing process is the same as the drawing process described in the magnetic wire manufacturing method described above, so a detailed description thereof will be omitted.
  • a first heat-treated material is produced by subjecting the drawn wire material to a first heat treatment.
  • the third step is the same as the second step in the magnetic wire manufacturing method described above.
  • the first heat treatment is the same as the first heat treatment described in the magnetic wire manufacturing method described above, so detailed description thereof will be omitted.
  • the first heat-treated material is twisted.
  • the third step is the same as the third step in the magnetic wire manufacturing method described above.
  • the amount of strain due to twisting in the manufacturing method of the composite magnetic wire is different from the amount of strain due to twisting in the manufacturing method of the magnetic wire described above.
  • the twisting may be performed under conditions such that the twisted surface of the first heat-treated material has a strain amount of 0.8 or more and 3.0 or less.
  • a composite magnetic wire with high output characteristics can be stably manufactured by twisting so that the strain amount is 0.8 or more and 3.0 or less.
  • the strain amount may be 1.0 or more and 2.0 or less.
  • the composite magnetic wire 2 shown in FIG. 4 is regarded as the first heat-treated material.
  • the first heat-treated material is called "wire".
  • the method of obtaining the strain amount of the composite magnetic wire differs from the method of obtaining the strain amount described in the magnetic wire manufacturing method described above in that the strain amount is obtained using the diameter of the wire including the coating material.
  • Other points are the same as the twisting process described in the manufacturing method of the magnetic wire described above, so detailed description thereof will be omitted.
  • a twisted composite magnetic wire when twisting the first heat-treated material, if the twisting process is completed while the first heat-treated material is twisted, a twisted composite magnetic wire can be produced. For example, by rotating the first heat-treated material in only one direction, a twisted composite magnetic wire can be obtained. Alternatively, when the first heat-treated material is rotated clockwise and counterclockwise, the total number of rotations in the clockwise direction and the total number of rotations in the counterclockwise direction are different, so that the twisted composite A magnetic wire is obtained.
  • the conditions for twisting may be appropriately selected so that the angle ⁇ t of the twist mark 50 shown in FIG. 6 falls within the above-described specific range. Specifically, twist processing may be performed so that the angle ⁇ t of the twist mark 50 is 4° or more and 60° or less.
  • the method for manufacturing a composite magnetic wire according to the embodiment may include, after the fourth step of twisting, a step of subjecting the twisted first heat-treated material to a second heat treatment. Simultaneously with the step of performing, a step of subjecting the first heat treated material during twisting to a second heat treatment may be provided.
  • the step of performing the second heat treatment is the same as the step of performing the second heat treatment in the magnetic wire manufacturing method described above.
  • the second heat treatment is the same as the second heat treatment described in the magnetic wire manufacturing method described above, so detailed description thereof will be omitted.
  • the magnetic wire 1 and composite magnetic wire 2 of the embodiment can be suitably used for cores such as magnetic sensors, for example. Since the magnetic wire 1 and the composite magnetic wire 2 of the embodiment can provide a high output, it is possible to increase the output of the magnetic sensor. In addition, the magnetic wire 1 and the composite magnetic wire 2 of the embodiment can provide a high output and have a small variation in output, so stable output can be easily obtained even if the diameter or length is small. Therefore, it is possible to reduce the size of the magnetic sensor. Magnetic sensors can be used, for example, in magnetic encoders, motors, water meters, and the like.
  • a magnetic wire sample was produced by the magnetic wire production method described above.
  • a material made of an alloy having a composition shown in Table 1 was prepared.
  • the content of each element shown in Table 1 is a value when the total content of the elements contained in the alloy is 100% by mass.
  • "bal.” in the “Fe” column represents the balance.
  • the material is produced by vacuum melting an alloy and then hot-working it into a linear shape. The material diameter is 2.0 mm.
  • a drawn wire material was obtained by drawing the material.
  • the shape of the drawn wire is a round wire. That is, the drawn wire has a circular cross section.
  • the diameter of the drawn wire is 0.3 mm.
  • the total workability is 97.75%.
  • the drawing process was performed cold. Here, the drawing process was performed a plurality of times, and an intermediate heat treatment was performed during the drawing process.
  • the intermediate heat treatment was performed once when the material was drawn to a diameter of 0.6 mm. After the intermediate heat treatment, drawing was performed until the diameter of the drawn wire material reached 0.3 mm. After the intermediate heat treatment, the degree of working up to the final drawing was set to 75%.
  • the temperature of the intermediate heat treatment was 800°C.
  • the duration of the intermediate heat treatment was 60 minutes.
  • the intermediate heat treatment was performed under a hydrogen atmosphere.
  • the cooling rate after the intermediate heat treatment was set to 10° C./second or more.
  • the first heat treatment was performed on the drawn wire material.
  • the temperature of the first heat treatment was the temperature shown in Table 2.
  • the duration of the first heat treatment was 60 minutes.
  • a first heat treatment was performed in a hydrogen atmosphere. After performing the first heat treatment, the first heat-treated material subjected to the first heat treatment was cooled to room temperature.
  • the cooling rate after the first heat treatment was set to 10° C./second or more.
  • the first heat-treated material was twisted.
  • the first heat-treated material was cut to a length of 50 mm. Both ends of the cut first heat-treated material were gripped with chucks, and one of the chucks was rotated to twist the cut first heat-treated material. In this case, the first heat-treated material gripped by the chuck is twisted except for both ends.
  • the length of each end of the first heat-treated material to be gripped by the chuck was 10 mm so that the distance between the chucks was 30 mm.
  • the length of the portion excluding both ends of the first heat-treated material gripped by the chuck corresponds to the length L of the first heat-treated material to be twisted. That is, the length of the twisted portion is 30 mm.
  • the twisting was performed under conditions such that the strain amount on the surface of the twisted first heat-treated material was the strain amount shown in Table 2. Twisting was done cold. For example, sample no. As for the twisting condition 1, one set of twisting work was performed in the order of clockwise 6 rotations, counterclockwise 12 rotations, and clockwise 6 rotations, and this was repeated for 3 sets. Sample no. 101 to sample no. 103, and sample no. 107 was more susceptible to disconnection due to twisting than other samples, so it was difficult to twist to obtain a sufficient amount of strain. Sample no. 101 to sample no. 103, and sample no. 107 was twisted so that the strain amount was less than 1.0, specifically 0.5 or less. In Table 2, when the column of "strain amount" is " ⁇ 1.0", it indicates that the strain amount is less than 1.0.
  • the twisted first heat-treated material was cut to a length of 13 mm.
  • Sample no. In No. 4 the twisted first heat-treated material was subjected to the second heat treatment.
  • the temperature of the second heat treatment was 350°C.
  • the duration of the second heat treatment was 60 minutes.
  • Table 2 when the column of "2nd heat treatment presence/absence" is "absence”, it indicates that the second heat treatment was not performed, and when "yes", it indicates that the second heat treatment was performed.
  • the second heat-treated material subjected to the second heat treatment was cooled to room temperature.
  • the prepared magnetic wire sample is a round wire with a diameter of 0.3 mm and a length of 13 mm.
  • composition The magnetic wire composition of each sample was investigated using ICP emission spectroscopy.
  • the composition of the magnetic wire is substantially the same as the composition of the material, as shown in Table 1.
  • the magnetic wire texture of each sample was examined using SEM-EBSD. Specifically, the area ratio of the ⁇ phase, the KAM value of the ⁇ phase, the average crystal grain size of the ⁇ phase, the ratio of high-angle grain boundaries, and the ratio of ⁇ 3 grain boundaries were determined for the magnetic wire structure of each sample.
  • the magnetic wire is cut in a plane orthogonal to the length of the magnetic wire to obtain a cross section. Grind this cross-section.
  • the polished cross section is crystallographically analyzed by the EBSD method.
  • the size of the observation field for measuring the area ratio of the ⁇ phase, the average crystal grain size of the ⁇ phase, the ratio of high-angle grain boundaries, the ratio of ⁇ 3 grain boundaries, and the KAM value of the ⁇ phase is 11 ⁇ m ⁇ 34 ⁇ m.
  • SUPRA 35VP manufactured by Carl Zeiss was used as a measuring device.
  • the EBSD conditions were an electron beam acceleration voltage of 15 kV and an electron beam scanning interval of 0.05 ⁇ m.
  • OIM Analysis Version 7.3 manufactured by TSL Solutions Co., Ltd. was used as analysis software. In addition, data points with a confidence index of 0.1 or more in this analysis software were adopted.
  • Fig. 7 shows the sample No. obtained by the EBSD method.
  • Phase map The Phase map shown in FIG. 7 displays the ⁇ -phase in red and the ⁇ -phase in green. In FIG. 7, the red ⁇ -phase is displayed in dark gray, and the green ⁇ -phase is displayed in light gray.
  • FIG. 8 shows sample No. obtained by the EBSD method. 1 IQ map. In the IQ map shown in FIG. 8, a grain boundary having a crystal orientation difference of 15° or more is defined as a grain boundary.
  • ⁇ Area ratio of ⁇ phase> Based on the analysis results of the crystal structure obtained by the EBSD method, the area of the ⁇ phase and the area of the ⁇ phase within the observation field were measured. The B2 ordered phase was detected as the ⁇ phase. However, when the temperature range of the first heat treatment is higher than 750° C. and not higher than 850° C. and the second heat treatment is not performed, it is considered that almost no B2 ordered phase is formed.
  • the area ratio of the ⁇ -phase is calculated as the ratio obtained by dividing the area of the ⁇ -phase by the total area of the ⁇ -phase and the ⁇ -phase. The area ratio of the ⁇ -phase was determined as the average value of the area ratio of the ⁇ -phase for all of the above four observation fields.
  • Table 2 shows the measurement results of the ⁇ -phase area ratio. Also, the ratio of the total area of the ⁇ phase and the ⁇ phase within the observation field was obtained. The ratio of the total area of the ⁇ phase and the ⁇ phase is calculated as the ratio obtained by dividing the total area of the ⁇ phase and the ⁇ phase by the area of the observation field. The ratio of the total area of the ⁇ -phase and the ⁇ -phase was also taken as the average value in all the four observation fields. As a result, in all samples, the ratio of the total area of the ⁇ phase and the ⁇ phase was 98% or more.
  • ⁇ KAM value of ⁇ phase> Based on the crystal orientation analysis results obtained by the EBSD method, the KAM value of the ⁇ -phase in the observation field was measured. The KAM value of the ⁇ -phase was determined as the average value of the KAM values of the ⁇ -phase for all of the above four observation fields. Table 2 shows the measurement results of the ⁇ -phase KAM value.
  • ⁇ Average grain size of ⁇ phase> Based on the crystal orientation analysis results obtained by the EBSD method, the average crystal grain size of the ⁇ -phase in the observation field was measured.
  • a crystal grain boundary is defined as a crystal orientation difference of 15° or more between adjacent crystal grains.
  • the average crystal grain size of the ⁇ -phase was obtained by obtaining the area-weighted average diameter of the ⁇ -phase for all of the above four observation fields, and taking the average value thereof.
  • Table 2 shows the measurement results of the average crystal grain size of the ⁇ phase.
  • ⁇ Proportion of high-angle grain boundaries> Based on the crystal orientation analysis results obtained by the EBSD method, the crystal grain boundaries in the observation field were divided into high-angle grain boundaries and low-angle grain boundaries, and the lengths of the high-angle grain boundaries and the lengths of the low-angle grain boundaries were measured. .
  • a grain boundary with a crystal orientation difference of 15° or more is defined as a high-angle grain boundary
  • a grain boundary with a crystal orientation difference of 2° or more and less than 15° is defined as a small-angle grain boundary.
  • the sum of the length of the high-angle grain boundaries and the length of the low-angle grain boundaries is defined as the total length of the grain boundaries.
  • the high angle grain boundary fraction is calculated as the ratio of the length of the high angle grain boundary divided by the total length of the grain boundary.
  • the percentage of high-angle grain boundaries was calculated as the average value of the percentages of high-angle grain boundaries for all of the above four observation fields. Table 2 shows the measurement results of the proportion of high-angle grain boundaries.
  • ⁇ Ratio of ⁇ 3 grain boundaries> Based on the crystal orientation analysis results obtained by the EBSD method, the ⁇ 3 grain boundary was separated from the crystal grain boundary within the observation field, and the length of the ⁇ 3 grain boundary was measured. The ratio of ⁇ 3 grain boundaries is calculated as a ratio obtained by dividing the length of ⁇ 3 grain boundaries by the total length of the grain boundaries. The ratio of ⁇ 3 grain boundaries was obtained by obtaining the ratio of ⁇ 3 grain boundaries for all the observation fields of the above four points, and taking the average value thereof. Table 2 shows the measurement results of the ratio of ⁇ 3 grain boundaries.
  • Output characteristics The magnetic wire output characteristics of each sample were evaluated. Output characteristics are evaluated as follows. A coil component is produced by arranging a magnetic wire in a coil. An alternating magnetic field is applied from the outside of the coil component, and the pulse voltage generated in the coil is measured over time. The test conditions are as follows. Table 2 shows the measured pulse voltage as an output. Also, Table 2 shows variations in pulse voltage as coefficients of variation. However, sample no. 101 to sample no. 104, sample no. 107 and sample no. For 110, the coefficient of variation is not obtained.
  • the number of turns of the coil is 3000 turns.
  • the coil length is 10 mm.
  • - Prepare four magnets and a rotating disc.
  • the size of each magnet is 9 mm long ⁇ 5 mm wide ⁇ 2.5 mm thick.
  • Each of the four magnets is arranged on the rotating disk with a 90° shift around the central axis of the rotating disk.
  • the magnets are arranged in alternating polarities around the central axis of the rotating disk.
  • a rotating disk on which four magnets are arranged is rotated at a constant speed to generate an alternating magnetic field.
  • the magnetic field acting on the magnetic line is assumed to be this alternating magnetic field.
  • the higher the number of rotations of the rotating disk the higher the pulse voltage generated in the coil.
  • the distance between the side of the coil and the side of the magnet is 8 mm.
  • the rotation speed of the rotating disc is 60 rpm (revolutions per minute).
  • the pulse voltage was obtained as follows. The pulse voltage is measured until the total number of pulses reaches 2000 pulses. That is, the positive pulse voltage and the negative pulse voltage are measured until the number of positive pulse voltages and the number of negative pulse voltages reach 1000 pulses, respectively. The difference between the average value of the positive pulse voltage and the average value of the negative pulse voltage was determined and used as the pulse voltage. Furthermore, the variation coefficient of the pulse voltage was obtained. The coefficient of variation of the pulse voltage is an index representing variations in output. The smaller the variation coefficient of the pulse voltage, the smaller the output variation.
  • the coefficient of variation of the pulse voltage is the value obtained by dividing the standard deviation of the positive pulse voltage by the average value of the positive pulse voltage and expressed as a percentage.
  • a stable output can be obtained when the coefficient of variation is 7% or less.
  • the coefficient of variation may be 6% or less, or even 5% or less.
  • the magnetic wire No. 13 has an output of 15 V or more and is excellent in output characteristics. Furthermore, sample no. 1 to sample no. The magnetic wire No. 13 has a coefficient of variation of 7% or less, and has a small variation in output. Sample no. 1 to sample no. All 13 magnetic wires have a specific texture. Specifically, the structures of these magnetic wires satisfy all of the following three requirements. The area ratio of ⁇ phase is 90% or more, the average crystal grain size of ⁇ phase is 2.5 ⁇ m or less, and the ratio of high-angle grain boundaries is 60% or more. Furthermore, in addition to the above three requirements, the texture of these magnetic wires satisfies both the ratio of ⁇ 3 grain boundaries of 5% or more and the KAM value of the ⁇ phase of 0.45° or more.
  • sample No. 101 to sample no. The magnetic wire of No. 110 has an output of less than 15 V, and the sample No. 1 to sample no. The output characteristics are inferior to those of No. 13 magnetic wires.
  • sample no. 101 to sample no. All the textures of the magnetic wires of 103 have a small proportion of high-angle grain boundaries and a small proportion of ⁇ 3 grain boundaries.
  • a magnetic wire with a specific structure can obtain a high output and a stable output.
  • test results show the following. (1) No. 1 to No. From the comparison of 3, the larger the amount of strain due to twisting, the easier it is to obtain a high output.
  • V content is preferably 2% by mass or more, particularly preferably 5% by mass or more.
  • the upper limit of the V content is preferably 12% by mass.
  • the inclusion of Co in a specific range improves the output characteristics. From this result, it is considered that the Co content is preferably 40% by mass or more and 70% by mass or less. Also, No. From the results of No. 110, if the Co content is too high, a specific structure may not be obtained, and the output characteristics may deteriorate.
  • the Si content is preferably 0.1% by mass or more, more preferably 0.2% by mass or more.
  • the Ti content is preferably 0.05% by mass or more, more preferably 0.08% by mass or more.
  • the content of Al is considered to be preferably 0.2% by mass or more, more preferably 0.3% by mass or more.
  • the content of Mn is considered to be preferably 0.2% by mass or more, more preferably 0.4% by mass or more.
  • the KAM value of the ⁇ phase is preferably 0.47° or more, more preferably 0.50° or more.
  • the reason why the ⁇ -phase KAM value in No. 107 is small is considered to be that the amount of strain due to twisting is small.
  • the KAM value of the ⁇ phase in No. 11 is 1 to No.
  • the reason why the KAM value is smaller than the ⁇ -phase KAM value in No. 10 is considered to be that the temperature of the first heat treatment is relatively high. From this result, it is considered that the temperature of the first heat treatment is preferably 840° C. or lower, more preferably 820° C. or lower in the case of the composition shown in Table 1.
  • the reason why the ratio of high-angle grain boundaries and the ratio of ⁇ 3 grain boundaries in 103 is small is that the temperature of the first heat treatment is low, so that the ⁇ phase does not transform during the heat treatment and martensite transformation does not occur during cooling. . No. 102 and no.
  • the reason why the average crystal grain size of the ⁇ phase in 103 is large is considered to be due to recrystallization. No. 103 and no.
  • the reason why the area ratio of the ⁇ phase in 104 is small is considered to be that the first heat treatment caused V to segregate in the ⁇ phase and stabilize the ⁇ phase. From the above, it is considered that the temperature of the first heat treatment is preferably higher than 750° C., more preferably 760° C. or higher, in the case of the composition shown in Table 1. No. 6, the temperature of the first heat treatment is considered to be 780° C. or higher, more preferably 790° C. or higher.
  • Test Example 2 In Test Example 2, magnetic wire samples different from those in Test Example 1 in at least one of the diameter and length were produced.
  • Test Example 2 a material made of an alloy having the composition shown in Table 3 was prepared.
  • the material diameter is 2.0 mm.
  • Sample No. 21 and sample no. 22 differs from Test Example 1 in the diameter of the magnetic wire.
  • Sample no. 21 made the diameter of the wire drawing material 0.2 mm.
  • Sample no. The total working ratio of drawing in 21 is 99%.
  • Sample no. In 21, after the intermediate heat treatment, the degree of working up to the final drawing is 89%.
  • Sample no. 22 made the diameter of the wire drawing material 0.55 mm. Sample no. The total working ratio of drawing at 22 is 92%.
  • intermediate heat treatment was performed once at the stage where the material was drawn to a diameter of 0.6 mm.
  • Sample no. In 22, after the intermediate heat treatment, the degree of working up to the final drawing is 16%.
  • Test Example 2 the temperature of the first heat treatment was the temperature shown in Table 4.
  • the twisting process was performed under conditions such that the strain amount shown in Table 4 was obtained.
  • the twisted first heat-treated material was cut.
  • Sample no. At 21, the first heat treated material was cut into 13 mm lengths.
  • Sample no. 22 to sample no. No. 25 differs from Test Example 1 in the length of the magnetic wire.
  • Sample no. At 22, the first heat treated material was cut to 10 mm.
  • Sample no. At 23, the first heat treated material was cut to 7 mm.
  • Sample no. At 24, the first heat treated material was cut to 8.5 mm.
  • composition of the magnetic wire of each sample was investigated using ICP emission spectrometry.
  • the composition of the magnetic wire is substantially the same as the composition of the material, as shown in Table 3.
  • the structure of the magnetic wire of each sample was examined using SEM-EBSD. As in Test Example 1, the area ratio of the ⁇ phase, the KAM value of the ⁇ phase, the average crystal grain size of the ⁇ phase, the ratio of high-angle grain boundaries, and the ratio of ⁇ 3 grain boundaries were obtained. Table 4 shows the results.
  • the magnetic wire No. 25 has an output of 15 V or more and a coefficient of variation of 7% or less, and has high output characteristics.
  • Sample no. 21 to sample no. 25 magnetic wires are sample No. 1 of Test Example 1 shown in Table 2. 1 to sample no. Like 13, it has a specific organization. Sample no. 21 has sufficient output characteristics even if the diameter of the magnetic wire is small. Sample no. 23 has sufficient output characteristics even if the length of the magnetic wire is short. From this test result, it can be seen that a magnetic wire having a specific structure can ensure sufficient output characteristics even if the size is small.
  • a sample of the composite magnetic wire was produced by the method for manufacturing the composite magnetic wire described above.
  • sample No. 1 of Test Example 1 is used.
  • a core material made of an alloy having the same composition as that of No. 1 and a core material made of an Fe-65Ni alloy were prepared.
  • the core material of 111 is made of FeCoV alloy.
  • the core material of 112 is made of Fe-65Ni alloy.
  • the Fe-65Ni alloy is an alloy containing 65% by mass of Ni and the balance being Fe and unavoidable impurities.
  • the melting point of Fe-65Ni is 1250°C.
  • Table 5 shows the melting points of the alloys forming the core material.
  • the core material is produced by vacuum-melting an alloy and then hot-working it into a linear shape.
  • the shape of the core material is a round wire. That is, the shape of the cross section of the core material is circular.
  • a covered wire was obtained by covering the outer peripheral surface of the core material with a covering material.
  • a coating material made of metal shown in Table 5 was used for coating.
  • the material of the covering material is either SUS304L, SUS316L, permalloy B, nichrome, phosphor bronze, or FeCoV alloy.
  • Table 5 shows the melting points of the metals forming the coating material.
  • the covering material of 111 is made of SUS316L.
  • the coating material of 46 consists of SUS304L.
  • the cladding material of 47 consists of nichrome.
  • the cladding at 48 consists of Permalloy B. Sample no.
  • the cladding material of 112 consists of FeCoV alloy.
  • the composition of the coating material made of the FeCoV alloy contains 52% by mass of Co, 10% by mass of V, and the balance of Fe and unavoidable impurities.
  • the melting point of this FeCoV alloy is about 1300.degree.
  • the coating material was coated on the outer peripheral surface of the core material by a clad method. Specifically, the coating material was clad on the outer peripheral surface of the core material by inserting the core material into the pipe made of metal constituting the coating material and pulling it out.
  • the inner diameter of the pipe is about 2.1 mm.
  • the thickness of the pipe was adjusted so that the ratio of the core material was the value shown in Table 6 in the sample of the composite magnetic wire.
  • a drawn wire material was obtained by drawing the covered wire material.
  • the shape of the drawn wire is a round wire. That is, the drawn wire has a circular cross section.
  • the diameter of the drawn wire is 0.3 mm or 0.4 mm.
  • Sample no. 49 the diameter of the drawn wire is 0.4 mm.
  • Sample no. In samples other than 49 the diameter of the drawn wire is 0.3 mm.
  • the total workability is over 97.75%.
  • the drawing process was performed cold. Here, the drawing process was performed a plurality of times, and an intermediate heat treatment was performed during the drawing process. The intermediate heat treatment was performed once when the coated wire rod was drawn to a diameter of 0.6 mm. After the intermediate heat treatment, drawing was performed until the diameter of the drawn wire material reached 0.3 mm.
  • the degree of working up to the final drawing was set to 75%.
  • the temperature of the intermediate heat treatment was 800°C.
  • the duration of the intermediate heat treatment was 60 minutes.
  • the intermediate heat treatment was performed under a hydrogen atmosphere.
  • the cooling rate after the intermediate heat treatment was set to 10° C./second or more.
  • the first heat treatment was performed on the drawn wire material.
  • the temperature of the first heat treatment was the temperature shown in Table 6.
  • the duration of the first heat treatment was 60 minutes.
  • a first heat treatment was performed in a hydrogen atmosphere. After performing the first heat treatment, the first heat-treated material subjected to the first heat treatment was cooled to room temperature.
  • the cooling rate after the first heat treatment was set to 10° C./second or more.
  • the first heat-treated material was twisted.
  • the twisting method is the same as in Test Example 1. Twisting was performed under conditions that gave the amount of strain shown in Table 6. Moreover, sample no. 31 to sample no. 49, sample no. 111 and sample no. At 112, the twisting process is completed with the first heat treated material twisted. Specifically, when twisting the first heat-treated material, the total number of rotations clockwise and the total number of rotations counterclockwise were adjusted to be different.
  • the twisted first heat-treated material was cut into lengths of 13 mm or 10 mm.
  • Sample no. 49 was cut to a length of 10 mm.
  • Sample no. Samples other than 49 were cut to a length of 13 mm.
  • Sample no. No. 36 performed the second heat treatment on the twisted first heat treated material.
  • the temperature of the second heat treatment was 300°C.
  • the duration of the second heat treatment was 60 minutes.
  • Table 6 when the column "whether or not the second heat treatment was performed" is "absent", it indicates that the second heat treatment was not performed, and when it is "yes", it indicates that the second heat treatment was performed. After performing the second heat treatment, the second heat-treated material subjected to the second heat treatment was cooled to room temperature.
  • the prepared composite magnetic wire sample is sample No. Except for 49, they are round wires with a diameter of 0.3 mm and a length of 13 mm. Sample no.
  • the composite magnetic wire of 49 is a round wire with a diameter of 0.4 mm and a length of 10 mm.
  • Sample No. 1a and sample no. A magnetic wire of 1b was produced.
  • Sample no. 1a and sample no. 1b is sample No. 1 of Test Example 1; Like 1, it does not have a covering material.
  • Sample no. 1a and sample no. 1b is the same as sample No. 1b, except that the twisting conditions in the manufacturing process are different. It was prepared in the same manner as in 1.
  • the composition of the magnetic wire of sample No. 1b is as follows. It is substantially the same as the composition of the magnetic wire of 1.
  • Sample no. 1a and sample no. For 1b the first heat-treated material was subjected to twisting under conditions that gave the amount of strain shown in Table 6. However, sample no. 1a and sample no.
  • sample no. 1a and sample no. 1b is a twisted magnetic wire.
  • the magnetic wire in a twisted state has twist marks on the outer peripheral surface of the magnetic wire.
  • Sample no. 1a and sample no. 1b means that when the first heat-treated material is twisted, the total number of clockwise and counterclockwise rotations is the same, but the clockwise and counterclockwise rotations are the same. difference is different.
  • the composition of the core material in the composite magnetic wire of each sample was investigated using the EDX method.
  • the composition of the core material in 111 is the same as that of sample No. 1 of Test Example 1.
  • the composition was substantially the same as that of the magnetic wire of No. 1.
  • the material of the core material in 112 was Fe-65Ni alloy.
  • the composition of the coating material was analyzed using the EDX method, and the material of the coating material was as shown in Table 6.
  • the Vickers hardness of each of the core material and the coating material was determined. Each Vickers hardness was obtained by the method described in the above item " ⁇ Method for measuring Vickers hardness>". Table 6 shows the results. Moreover, sample no. 1, sample no. 1a and sample no. The Vickers hardness was also obtained for each magnetic wire of 1b. The Vickers hardness of the magnetic wire was obtained in the same manner as the Vickers hardness of the core material. The results are also shown in Table 6.
  • the melting point of the coating material was determined for the composite magnetic wire of each sample.
  • the melting point of the coating material was obtained by the method described in the above item " ⁇ Measuring method of melting point>".
  • the melting point of the coating material was the same as the melting point shown in Table 5.
  • Table 6 shows the ratio of the core material in the composite magnetic wire of each sample.
  • the ratio of the core material was determined as follows. The cross section of the composite magnetic wire was observed with an optical microscope to determine the diameter of the core material and the diameter of the composite magnetic wire. The ratio of the core material was obtained by dividing the diameter of the core material by the diameter of the composite magnetic wire.
  • Table 6 shows the twist trace angle in the composite magnetic wire of each sample.
  • the angle of the twist mark was determined as follows. The outer peripheral surface of the coating material was observed with an optical microscope to measure the inclination angle of the twist marks with respect to the axis of the composite magnetic wire. The angle of the twist marks was obtained by measuring the inclination angles of 20 or more twist marks and averaging the values. Sample no. 1a and sample no. For each magnetic wire of 1b, the angle of the twist mark was obtained. The angle of the twist mark of each magnetic wire was determined as follows. The outer peripheral surface of the magnetic wire was observed with an optical microscope to measure the angle of inclination of the twist mark with respect to the axis of the magnetic wire. Similar to the sample of the composite magnetic wire, the inclination angles of 20 or more twist marks were measured, and the average value was obtained. Sample no. 1a and sample no. Table 6 shows the twist trace angles in each magnetic wire of 1b.
  • Sample no. 31 to sample no. 49 composite magnetic wires have an output of 24 V or more.
  • Sample no. 31 to sample no. All the core materials of the composite magnetic wires of No. 49 are Sample Nos. 1, it has a specific texture.
  • the structure of the core material in these composite magnetic wires satisfies all of the following three requirements.
  • the area ratio of ⁇ phase is 90% or more
  • the average crystal grain size of ⁇ phase is 2.5 ⁇ m or less
  • the ratio of high-angle grain boundaries is 60% or more.
  • the structure of the core material satisfies both the above-mentioned three requirements and the ratio of ⁇ 3 grain boundaries of 5% or more and the KAM value of the ⁇ phase of 0.45° or more.
  • the ratio of the core material in No. 49 composite magnetic wire is 45% or more and 95% or less.
  • the composite magnetic wire of No. 111 is the sample No. 1, sample no. 1a and sample no.
  • the output is lower than each magnetic wire in 1b.
  • the composite magnetic wire No. 49 has a coefficient of variation of 7% or less, and a small variation in output. Sample no. 49 has sufficient output characteristics even if the length of the composite magnetic wire is short.
  • sample no. The composite magnetic wire of No. 112 has a coefficient of variation of more than 7% and a large variation in output. Sample no. 112 has an output of less than 15 V, sample No. 31 to sample no. Output characteristics are inferior to 49.
  • the core material of the composite magnetic wire of 112 does not have the specific structure mentioned above. Specifically, sample no. In the structure of the core material in the composite magnetic wire No. 112, the proportion of high-angle grain boundaries is less than 60%, and the proportion of ⁇ 3 grain boundaries is less than 5%.
  • test results show the following. (1) No. 31 to No. 33, No. 41 and no. 45 is twisted so that the amount of strain is equal. In addition, these samples have the same coating material. No. 31 to No. From the comparison of No. 33, it is easy to obtain a high output when the ratio of the core material is small to some extent. It is believed that the upper limit of the ratio of the core material is preferably 95%, more preferably 90%, and particularly preferably 85%. No. 41 and no. 45, it is easy to obtain high output when the ratio of the core material is large to some extent.
  • the lower limit of the ratio of the core material is considered to be preferably 48%, more preferably 55%, and particularly preferably 60%.
  • Stainless steel is considered to be preferable as the material of the covering material.
  • the Vickers hardness of the covering material is considered to be preferably 300 HV or more.
  • [Appendix 1] a step of drawing a core material made of an alloy containing iron and cobalt as main components to obtain a drawn wire; a step of subjecting the drawn wire material to a first heat treatment to obtain a first heat treated material; obtaining a coated wire by coating the outer peripheral surface of the first heat-treated material with a coating; A step of twisting the coated wire, In the first heat treatment, the structure of the alloy of the core material in the first heat-treated material contains an ⁇ phase and a ⁇ phase, and the ⁇ Performed under conditions such that the area ratio of the phase is 90% or more, A manufacturing method of a composite magnetic wire.
  • the method for producing a composite magnetic wire described in Supplementary Note 1 can produce a composite magnetic wire with excellent output characteristics.
  • the reason for this is that the first heat treatment controls the structure of the core material in the first heat-treated material so that it becomes a specific structure in which the ⁇ phase and the ⁇ phase coexist.
  • a composite magnetic wire with high output characteristics can be obtained by twisting the first heat-treated material.
  • twisting is performed in a state in which the core material is covered with the covering material.
  • the core material is pulled by the covering material in the vicinity of the outer peripheral surface of the core material, and the core material is elongated along the length of the core material.
  • the twisting introduces a tensile residual stress into the core along the length of the core.
  • the tensile residual stress increases and the uniaxial anisotropy of the core material increases. Since the uniaxial anisotropy of the core material is increased, the output characteristics of the core material are improved.
  • the method for manufacturing a composite magnetic wire described in appendix 1 differs from the method for manufacturing a composite magnetic wire according to the above-described embodiment in that the first heat treatment is performed before coating with the coating material.
  • the steps proceed in the order of [wire drawing] ⁇ [first heat treatment] ⁇ [coating] ⁇ [twisting].
  • the first heat treatment is performed after drawing the core material. After performing the first heat treatment, the first heat-treated material is covered with a coating material.
  • the steps proceed in the order of [coating] ⁇ [wire drawing] ⁇ [first heat treatment] ⁇ [twisting].
  • the core material is first coated with the coating material. After the coated wire is drawn, a first heat treatment is performed. That is, in the manufacturing method of appendix 1, the core material is not coated with the coating material in the step of performing the first heat treatment. Since the first heat treatment is performed without covering the core material with the covering material, the melting point of the covering material may be lower than the temperature of the first heat treatment. The melting point of the coating material may be 850° C. or less. In the case of the manufacturing method of appendix 1, a metal having a lower melting point than the coating material used in the manufacturing method of the embodiment can be used as the coating material.
  • the covering material may be formed by a plating method.
  • the compressive strain does not occur in the first heat-treated material, so that the output characteristics of the core material are hardly affected.
  • the covering material is formed by the clad method, compressive strain occurs in the first heat-treated material, which may affect the output characteristics of the core material.
  • the coating process is performed after the wire drawing process, no traces of wire drawing remain on the surface of the coated wire.
  • the surface of the covered wire is deformed, thereby forming streaky twist marks on the surface of the covered wire. Therefore, the composite magnetic wire obtained by the manufacturing method of Supplementary Note 1 has twist marks, like the composite magnetic wire obtained by the manufacturing method of the embodiment.
  • Appendix 2 The method for producing a composite magnetic wire according to appendix 1, wherein the step of twisting is performed under conditions such that the amount of strain on the surface of the coated wire that has been subjected to the twisting is 0.8 or more and 3.0 or less. .
  • a composite magnetic wire with high output characteristics can be stably manufactured.
  • the reason why the twisting is performed under the condition that the strain amount is 0.8 or more and 3.0 or less is the same as in the manufacturing method of the composite magnetic wire according to the embodiment described above.
  • Appendix 3 After the twisting step, the twisted covered wire is subjected to a second heat treatment, or simultaneously with the twisting step, the twisted covered wire is subjected to a second heat treatment. Equipped with a process, The method for manufacturing a composite magnetic wire according to Appendix 1 or Appendix 2, wherein the second heat treatment is performed by heat-treating the coated wire after the twisting process or the coated wire during the twisting process at a temperature of 150° C. or more and 400° C. or less. .
  • the output characteristics of the composite magnetic wire can be enhanced.
  • the reason for performing the second heat treatment is the same as in the manufacturing method of the composite magnetic wire according to the embodiment described above.
  • Appendix 4 3. The method for producing a composite magnetic wire according to any one of appendices 1 to 3, wherein the first heat treatment heat-treats the drawn wire material at a temperature higher than 750°C and not higher than 850°C.
  • Appendix 5 The method for producing a composite magnetic wire according to any one of appendices 1 to 4, wherein the step of obtaining the drawn wire includes a step of drawing the core material at a workability of 10% or more.

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PCT/JP2022/039747 2021-11-01 2022-10-25 磁性線、複合磁性線、磁性線の製造方法、及び複合磁性線の製造方法 Ceased WO2023074693A1 (ja)

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DE112022005236.8T DE112022005236T5 (de) 2021-11-01 2022-10-25 Magnetischer Draht, zusammengesetzter magnetischer Draht, Verfahren zur Herstellung eines magnetischen Drahtes und Verfahren zur Herstellung eines magnetischen Verbunddrahtes
JP2023556467A JPWO2023074693A1 (https=) 2021-11-01 2022-10-25
CN202280072410.XA CN118176313A (zh) 2021-11-01 2022-10-25 磁性线、复合磁性线、磁性线的制造方法、以及复合磁性线的制造方法
US18/704,880 US20250257428A1 (en) 2021-11-01 2022-10-25 Magnetic wire, composite magnetic wire, method for manufacturing magnetic wire, and method for manufacturing composite magnetic wire

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