EP2697399A1 - Alliage, noyau magnétique et procédé pour fabriquer une bande d'un alliage - Google Patents

Alliage, noyau magnétique et procédé pour fabriquer une bande d'un alliage

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Publication number
EP2697399A1
EP2697399A1 EP12720963.3A EP12720963A EP2697399A1 EP 2697399 A1 EP2697399 A1 EP 2697399A1 EP 12720963 A EP12720963 A EP 12720963A EP 2697399 A1 EP2697399 A1 EP 2697399A1
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EP
European Patent Office
Prior art keywords
atom
alloy
permeability
less
heat treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP12720963.3A
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German (de)
English (en)
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EP2697399B1 (fr
Inventor
Giselher Herzer
Christian Polak
Viktoria BUDINSKY
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Vacuumschmelze GmbH and Co KG
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Vacuumschmelze GmbH and Co KG
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Classifications

    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/04—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering with simultaneous application of supersonic waves, magnetic or electric fields
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • 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 by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties 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 by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • 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 by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • 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
    • C22C38/12—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
    • C22C45/00—Amorphous alloys
    • C22C45/02—Amorphous alloys with iron as the major constituent
    • 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
    • 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
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • 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
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
    • 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
    • H01F41/02—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 for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0213—Manufacturing of magnetic circuits made from strip(s) or ribbon(s)
    • H01F41/0226—Manufacturing of magnetic circuits made from strip(s) or ribbon(s) from amorphous ribbons
    • 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
    • C21D2201/03—Amorphous or microcrystalline structure

Definitions

  • the present invention relates to an alloy, in particular a soft magnetic alloy suitable for use as a magnetic core, a magnetic core and a method for producing an alloy strip.
  • Nanocrystalline alloys based on a composition Feioo-a- b -cdxy- z Cu a Nb b M c T d Si x B y Z z can be used as a magnetic core for different applications.
  • the US 7,583,173 discloses a wound magnetic core which is used, inter alia, with a current transformer of (Fei_ a Ni a) ioo-x-y _ z _ a _ b _c CUxSiyBz baM 'M' ' ⁇ , wherein a ⁇ 0 , 3, 0.6 ⁇ x ⁇ 1.5, 10 ⁇ y ⁇ 17, 5 ⁇ z ⁇ 14, 2 ⁇ ⁇ 6, ⁇ ⁇ 7, ⁇ ⁇ 8, ⁇ 'at least one of the elements V, Cr, AI and Zn and M "are at least one of C, Ge, P, Ga, Sb, In and Be.
  • EP 0 271 657 A2 also discloses alloys with a summary on this basis.
  • These alloys also in the form of tapes, can be used as the magnetic core in various components, such as power transformers, current transformers and storage chokes.
  • the lowest possible production costs are generally desirable. However, the cost reduction should have as little or no effect on the operation of the magnetic core. In some applications of magnetic cores, further reduction of the size and weight of the magnetic core is desirable so that the size and weight of the component itself can be further reduced. At the same time, however, no increase in the manufacturing cost of the magnetic core is desired.
  • the object is therefore to provide an alloy which is suitable for use as a magnetic core, which can be produced more cheaply. Another object is to select the alloys so that the size and / or weight of the magnetic core can be reduced compared to a conventional magnetic core.
  • M is one or more of Mo
  • Ta or Zr is one or more of V
  • Z is one or more of C, P or Ge and 0 at% ⁇ a ⁇ 1.5 Atom%, 0 atom% ⁇ b ⁇ 2 atom%, 0 atom% ⁇ (b + c) ⁇ 2
  • the alloy is further formed in the form of a band and has a nanocrystalline structure in which at least 50% by volume of the grains have an average size of less than 100 nm.
  • the alloy also has a hysteresis loop with a central linear part, a remanence ratio, J T / J S , ⁇ 0.1, and a ratio of coercive field strength, H c , to anisotropic field strength, H a , ⁇ 10%.
  • the alloy thus has a composition with a niobium content of less than 2 atomic percent.
  • This has the advantage that the raw material costs are lower compared to a composition with a higher niobium content, since niobium is a relatively expensive element.
  • the lower limit of the silicon content and the upper limit of the boron content of the alloy are determined so that the alloy can be made in the form of a strip under tension in a continuous furnace, thereby achieving the above-mentioned magnetic properties.
  • the alloy may also exhibit the desired soft magnetic properties for magnetic core applications.
  • the shape as a band not only makes it possible to manufacture the alloy under tension in a continuous furnace, but also to manufacture a magnetic core having any number of windings. Consequently, the size and magnetic properties of the magnetic core can be easily adjusted by appropriate selection of the windings to the application. Due to the nanocrystalline structure with a particle size of less than 100 nm in at least 50% by volume of the alloy, a low saturation magnetostriction is achieved at high saturation polarization. Due to the heat treatment under tensile stress, a suitable magnetic alloy selection results in a magnetic hysteresis loop with a central linear part, a remanence ratio of less than 0.1 and a coercive field strength of less than 10% of the anisotropy field.
  • the central part of the hysteresis loop is defined as the part of the hysteresis loop that lies between the anisotropy field strength points that characterize the transition to saturation.
  • 5J on or 5J ab denote the standard deviation of the magnetization from a compensation straight line by the rising or rising branch of the hysteresis loop between magnetization values of + 75% of the saturation polarization J s .
  • This alloy is therefore particularly suitable for a magnetic core having a reduced size and a smaller weight with lower raw material costs and at the same time the desired soft magnetic properties for use as a magnetic core.
  • the remanence ratio of the alloy is less than 0.05.
  • the hysteresis loop of the alloy is thus even more linear or flat.
  • the ratio of coercive strength to anisotropic field strength is less than 5%.
  • the hysteresis loop even more linear, so that the Ummagnetleitershnee are even lower.
  • the alloy further has a permeability ⁇ of 40 to 3000 or 80 to 1500.
  • the alloy has a permeability between about 200 and 9000. In these and other examples, the permeability is determined primarily by the choice of tensile stress in the heat treatment. The tensile stress can be up to about 800 MPa without the band breaking.
  • Such relatively low permeabilities are advantageous for current transformers, power transmitters, storage chokes, and other applications where the magnetic core should not be ferromagnetic saturated so that the inductance does not suffer losses when high electrical currents flow through windings around the magnetic core.
  • Suitable permeability ranges result from the specific requirements of the respective application. Suitable ranges are 1500 to 3000, 200 to 1500 and 50 to 200. Thus, for example, a permeability ⁇ of about 1500 to about 3000 is advantageous for DC-tolerant current transformers, while for power transmitters a permeability range of about 200 to 1500 and for storage chokes rather a permeability range from about 50 to 200 is particularly suitable.
  • the alloy may have a saturation magnetostriction of less than 5 ppm in magnitude. Alloys with a saturation magnetostriction below these limits have particularly good soft magnetic properties even with internal stress, especially when the permeability is not significantly greater than 500. For higher permeabilities it is advantageous to select alloys with smaller values of saturation magnetostriction.
  • the alloy may also have a saturation magnetostriction of less than 2 ppm, preferably less than 1 ppm. Alloys with a saturation magnetostriction below these limits have particularly good soft-magnetic properties, even with internal stress, in particular if the permeability ⁇ is greater than 500 or greater than 1000.
  • the alloy comprises niobium and / or copper, where 0 ⁇ a ⁇ 0.5 and 0 ⁇ b ⁇ 0.5.
  • the silicon content and / or the boron content is further defined such that the alloy has 14 atom% ⁇ x ⁇ 17 atom% and / or 5.5 atom% ⁇ y ⁇ 8 atom%.
  • the alloy has the shape of a band.
  • This band may have a thickness of 10 ⁇ to 50 ⁇ . This thickness makes it possible to wind a magnetic core with a large number of windings, which at the same time has a small outer diameter.
  • At least 70 vol-% of the grains have a mean size of less than 50 nm. This allows a further increase in the magnetic properties.
  • the alloy is heat-treated in the form of a ribbon under tension to produce the desired magnetic properties.
  • the alloy ie the finished heat-treated strip, is thus also characterized by a structure which originated by this manufacturing process.
  • the crystallites have an average size of about 20-25 nm and a remanent elongation in the tape longitudinal direction between about 0.02% and 0.5%, which is proportional to the tensile stress applied during the heat treatment. For example, a heat treatment under a tensile stress of 100 MPa results in an elongation of about 0.1%.
  • the crystalline grains may have an elongation of at least 0.02% in a preferred direction.
  • the magnetic core may be in the form of a wound tape, wherein to form the magnetic core, depending on the application, the tape may be wound in a plane or as a solenoid about an axis.
  • the band of the magnetic core may be coated with an insulating layer to electrically insulate the windings of the magnetic core from each other.
  • the layer may be, for example, a polymer layer or a ceramic layer.
  • the tape may be coated with the insulating layer before and / or after winding into a magnetic core.
  • the magnetic core according to one of the preceding embodiments can be used in various components.
  • a power transformer, a current transformer and a storage choke with a magnetic core according to one of these exemplary embodiments are also specified.
  • a method for producing a tape is also disclosed, comprising: providing an amorphous alloy tape having a composition consisting of
  • M is one or more of the elements Mo, Ta, or Zr, a T or more of the elements V, Mn, Cr, Co or Ni and Z, one or more of the elements C, P or Ge and 0 atom% ⁇ a ⁇ 1.5 atom%, 0 atom% ⁇ b ⁇ 2 atom%, 0 atom % ⁇ (b + c) ⁇ 2 atom%, 0 atom% ⁇ d ⁇ 5 atom%, 10 atom% ⁇ x ⁇ 18 atom%, 5 atom% ⁇ y ⁇ 11 atom% and 0 atom% ⁇ z ⁇ 2 atom % is.
  • Tape is heat treated under tension in a continuous oven at a temperature T a , where 450 ° C ⁇ Ta ⁇ 750 ° C.
  • This composition can be prepared with a heat treatment between 450 ° C and 750 ° C under tension with suitable magnetic properties for use as a magnetic core.
  • the heat treatment results in the formation of a nanocrystalline microstructure in which at least 50% by volume of the grains have an average size smaller than 100 nm.
  • this composition with less than 2 atomic percent of niobium can be made by this method to have a hysteresis loop with a central linear part, a remanence ratio, J r / J s , ⁇ 0.1, and a coercive-field strength, H c , to anisotropic field strength, H a , ⁇ 10%.
  • the strip is heat treated in the pass. Consequently, the belt is pulled through the continuous furnace at a speed s.
  • This speed s can be set so that a residence time of the belt in a temperature zone of the belt
  • Continuous furnace with the temperature within 5% of the T a is between 2 seconds and 2 minutes.
  • the time to heat the tape to the temperature T a is of a comparable order of magnitude as the duration of the heat treatment itself. The same applies to the duration of the subsequent cooling.
  • This residence time leads in this tempering temperature range to the desired structure and the desired magnetic properties.
  • the tape is pulled through the continuous furnace under a tension of between 5 and 160 MPa.
  • the band is pulled through the continuous furnace under a tensile stress of 20 MPa to 500 MPa. It is also possible to pull the strip through the kiln even with a higher tensile stress up to about 800 MPa without tearing it. This range of tensile stress is suitable for achieving the desired magnetic properties in the abovementioned compositions.
  • the value of the permeability ⁇ achieved is inversely proportional to the tensile stress a a applied during the heat treatment.
  • a tensile stress ⁇ a is required which corresponds to the relation ⁇ 3 ⁇ ⁇ / ⁇ enough.
  • ⁇ has a value of ⁇ 48,000 MPa.
  • ⁇ has a value of, for example, ⁇ 36000 MPa.
  • values in the range of ⁇ 30,000 MPa to ⁇ ⁇ 700,000 MPa can be used for the alloys according to the invention and the corresponding heat treatment process. The exact value depends on the composition, the tempering temperature and to some extent on the tempering time.
  • the tensile stress that leads to the desired magnetic properties may therefore be dependent on the composition of the alloy and on the tempering temperature as well as the tempering time.
  • the ⁇ for a bene vorgege- permeability tensile stress required a a from the permeability is a UTest Testglühung out under a tension a Te st according to the relation
  • the desired magnetic properties may also be dependent on the tempering temperature T a and consequently set by the selection of the tempering temperature.
  • the temperature T a ⁇ (T x2 + 30 ° C) is selected for execution in an off depending on the niobium content B according to the relation (T xi + 50 ° C) ⁇ T a.
  • T xi and T x2 correspond to the crystallization temperatures defined by the maximum of the heat of transformation, which are determined by means of thermal standard methods such as DSC (differential scanning calometry) at a heating rate of 10 K / min.
  • a desired value of the permeability or anisotropic field strength, as well as a permitted deviation range is predetermined.
  • magnetic properties of the belt are continuously measured when leaving the continuous furnace.
  • the tension on the belt is adjusted accordingly to bring the measured values of the magnetic properties back within the allowable deviation ranges.
  • This embodiment reduces the deviations of the magnetic properties over the length of the band, so that the magnetic properties within a magnetic core are more homogeneous and / or the magnetic properties of a plurality of magnetic cores made from a single band deviate less.
  • the uniformity of the soft magnetic properties of the magnetic cores especially in commercial production, can be improved.
  • FIG. 1 shows a diagram of hysteresis loops of comparative examples of nanocrystalline Fe 77 -xCui b x Sii 5.5 B s .5 with different niobium content after heat treatment in a magnetic field transverse to the strip direction.
  • FIG. 1 shows a diagram of hysteresis loops of comparative examples of nanocrystalline Fe 77 -xCui b x Sii 5.5 B s .5 with different niobium content after heat treatment in a magnetic field transverse to the strip direction.
  • FIG. 2 shows a diagram of hysteresis loops of nanocrystalline Fe 7 7 - x Cui b x Sii 5.5 B s .5 after heat treatment under a tensile stress along the strip direction for different niobium contents
  • Figure 3 shows a diagram of the remanence ratio of nanocrystalline Fe 7 7 _ x Cui b x Sii 5.5 B s .5 after heat treatment in the magnetic field and after heat treatment Tensile stress as a function of Nb content
  • Figure 4 shows a diagram of the saturation polarization of
  • FIG. 5 shows a diagram of saturation magnetostriction
  • Figure 8 shows the X-ray diffraction patterns for the alloy
  • FIG. 9 shows a diagram of permeability ⁇ , anisotropy field Ha / coercive field strength H c , remanence ratio
  • Figure 10 shows the upper and lower optimum annealing temperature
  • FIG. 11 shows a diagram of coercive field strength H c
  • Figure 12 shows a graph of hysteresis loops of a LE Government Fe 8o SINB 9 and a comparative composition
  • FIG. 13 shows a schematic view of a continuous furnace.
  • Table 1 shows the nonlinearity factor NL for various
  • Table 2 shows measured temperatures and crystallization temperatures T a suitable occasion for annealing times of about 2s to 10s for different Nb contents of the alloy Fe 77 _ x x CuiNb Sii5.5B s .5,
  • Table 3 shows magnetic properties of an alloy
  • Table 5 shows in the production state measured saturation polarization J s , after heat treatment at different tempering temperatures T a measured values of
  • Table 6 shows in the manufactured measured saturation polarization J s, measured after heat treatment values of non-linearity NL, remanence J T / J S, Koerzi - tivfeidschreib H c, anisotropy field H a and relative permeability ⁇ of various alloy compositions
  • Table 7 shows the saturation magnetostriction A s of different Alloy compositions measured in the state of manufacture and after heat treatment under tension at the specified tempering temperature T a .
  • FIG. 1 shows a diagram of hysteresis loops of nanocrystalline alloys in the form of a band.
  • the bands have a composition of Fe 7 7_ x Cui x Sii 5 . 5 B s .5.
  • Figure 1 shows that with decreasing Nb content the hysteresis loops become non-linear. This nonlinear hysteresis loop is undesirable in some magnetic core applications because the core loss losses are increased.
  • Table 1 shows the nonlinearity factors NL of the hysteresis loops shown in Figs. 1 and 2 for various heat treatments and various Nb contents.
  • Table 1 shows the nonlinearity factor of nanocrystalline Fe 77 - x Cui b x Sii 5 . 5 B s .5 after heat treatment in a magnetic field for 0.5 h at a temperature of 540 ° C and after a heat treatment under tensile stress of 100 MPa for 4s at 600 ° C for various Nb contents.
  • Figure 3 shows a graph of remanence J r / 'J s heat-treated samples as a function of the Nb content.
  • Figure 3 shows the remanence ratio of nanocrystalline Fe 77 _ x x CuiNb Sii. 5 5 B s . 5 after heat treatment in a magnetic field of 0.5 h at temperatures of 480 ° C to 540 ° C and after heat treatment under tensile stress of 4 s at temperatures between 520 ° C and 700 ° C as a function of the Nb content.
  • linear loops with a remanence ratio smaller than 0.1 and a non-linearity factor smaller than 3% are reliably achieved only for Nb contents greater than 2 at%.
  • linear loops with a remanence ratio less than 0.1 and a nonlinearity factor less than 3% can be reliably achieved for Nb contents less than 2 at% and even for compositions without niobium.
  • Tables 1 to 6 and Figures 2 to 12 show that linear loops with a small remanence ratio at
  • compositions can be achieved with a niobium content of less than 2 atom%, when the heat treatment is carried out under a tensile stress in the tape longitudinal direction. These compositions have the advantage that raw material costs are reduced since niobium is a relatively expensive element.
  • FIG. 2 shows a diagram of hysteresis loops of bands after heat treatment in the course of an effective one
  • the time is defined at which the band passes through the temperature zone at which the temperature within 5% corresponds to the tempering temperature given here.
  • the time to heat the tape to the tempering temperature is comparable to the duration of the heat treatment itself. The same applies to the duration of the subsequent
  • FIG. 2 shows that for Nb contents of less than 2 at%, hysteresis loops with a central linear part and a small remanence ratio can be obtained.
  • the composition with Nb 3at% is a comparative example and the compositions with Nb ⁇ 2at% are examples according to the invention.
  • the arrow shows by way of example the definition of the anisotropy field strength H a .
  • FIG. 3 shows a graph of a remanence ratio comparison for such tension-tempered samples, shown in FIG. 3 with filled diamonds, and for magnetic field-annealed samples, shown with open circle symbols, as a function of Nb content.
  • Alloys with Nb contents below 2 at% have a small remanence ratio of less than 0.05 only when heat-treated under tension.
  • the remanence ratio is significantly higher, so that these alloys are not suitable for some magnetic core applications.
  • Even for the alloy Fe 77 CuiSii 5.5 B s .5, ie without addition of Nb a substantially linear loop with a remanence ratio of less than 0.05 results when heat-treated under a tensile stress.
  • FIG. 4 shows a diagram of the saturation polarization of alloys with a composition of Fe 7 7 - x Cu x b x Sii 5.5 B s .5 as a function of the Nb content.
  • the alloys with reduced Nb content have a significantly increased saturation polarization. This can be beneficial in a corresponding weight and Reduced manufacturing costs of the magnetic core can be implemented. Thus, in addition to reduced raw material costs, a further advantage results since the device having the magnetic core can be made smaller.
  • FIG. 5 shows a plot of saturation magnetostriction ⁇ ⁇ , anisotropy field H a , coercive field strength H c , remanence ratio J r / J s and nonlinearity factor NL of a composition Fe 75. 5 Cu 1 b 1 . 5 Si 15 .5B5.5 after heat treatment of about 4 seconds duration under a tensile stress of about 50 MPa as a function of the tempering temperature.
  • the anisotropy field H a field corresponds to that in which the linear portion of the hysteresis loop passes into the saturation shown in FIG.
  • the tempering temperatures between which the desired properties can be achieved, are in the range of about 535 ° C to 670 ° C, which is highlighted hatched in the figure.
  • the hatched area shows the area in which linear loops with small saturation magnetostriction, high anisotropy field and small remanence ratio result. This is also the area in which the alloys have particularly linear loops.
  • Figure 5 thus is the most suitable tempering temperature between 535 ° C and 670 ° C.
  • FIG. 6 shows the tempering behavior of a niobium-free alloy variant in which the optimum tempering temperatures are in the range of approximately 500 ° C. to 570 ° C., ie significantly lower than the composition of FIG. 5.
  • the optimum tempering temperatures according to the invention here are in the range of about 500 ° C to 570 ° C.
  • a flat linear hysteresis loop with a remanence ratio of less than 0.1 results.
  • FIG. 7 shows the crystallization behavior measured by means of differential scanning calometry (DSC) at a heating rate of 10 K / min using the example of the alloy Fe 77 CuiSii 5.5 B s .5.
  • DSC differential scanning calometry
  • FIG. 8 shows the X-ray diffraction diagrams for the alloy Fe 77 CuiSii 5.5 B s .5 in the amorphous initial state and after heat treatment under tension at different tempering temperatures in accordance with the different crystallization stages defined by T xi and T x2 .
  • FIG. 8 shows the X-ray diffraction pattern after a heat treatment under tension for 4s at 515 ° C, ie in the starting area, where magnetic properties according to the invention are achieved, and at 680 ° C, ie in the unfavorable starting area where no linear hysteresis loops with a small remanence ratio can be achieved more.
  • Alloy Fe 7 7CuiSii 5 .5B 6 .5 the average size of these crystallites is approximately in the range 38-44 nm. Performing an analogous analysis with the alloy composition Fe75.5Cu1 1.5Si15.5B6.5 by so obtained at the appropriate optimal occasion - Temperatures a mean crystallite size in the range 20-25 nm.
  • boride phases crystallize out of the amorphous residual matrix, which unfavorably influence the magnetic properties and lead to a non-linear loop with a high remanence ratio and high coercive strength.
  • T x i which corresponds to the crystallization of bcc-FeSi
  • T x2 which corresponds to the crystallization of borides
  • the suitable tempering temperature is approximately between T xi and T x2 and leads to a structure of nanocrystalline grains with a mean grain size less than 50 nm, which in an amorphous Embedded matrix, and the desired magnetic properties.
  • T xi and T x2 and the tempering temperatures T a depend on the heating rate and the duration of the heat treatment. Therefore, with a heat treatment time of less than 10 seconds, the optimum tempering temperatures at higher temperatures than the measured by differential scanning calorimetry (DSC) at 10K / min crystallization temperatures T xi and T x2 of Table 2. Accordingly, for longer tempering times, for example, 10 min up to 60 minutes, the optimum tempering temperatures T a typically 50 ° C to 100 ° C lower than the values of T a listed in Table 2 for a heat treatment time of a few seconds.
  • DSC differential scanning calorimetry
  • the tempering temperatures T a may be adjusted according to the composition and duration of the heat treatment according to the teaching of FIG. 5 and based on the crystallization temperatures measured in the DSC according to Table 2.
  • the crystallization temperatures measured at a heating rate of 10 K / min correspond approximately to the optimum starting range for an isothermal heat treatment lasting a few minutes.
  • FIG. 9 shows the dependence of the permeability, the anisotropy field, the coercive field strength, the remanence ratio and the nonlinearity factor on the tensile stress applied during the heat treatment.
  • FIG. 9 shows a diagram of the permeability, the anisotropy field, the coercive field strength, the remanence ratio and the nonlinearity factor of nanocrystalline
  • Table 4 shows another example of the dependence of the permeability, the anisotropy field, the coercive field strength, the remanence ratio and the nonlinearity factor on the tensile stress applied during the heat treatment.
  • the table shows the permeability, the anisotropy field, the coercive field strength, the remanence ratio and the nonlinearity factor of nanocrystalline
  • FIG. 9 and Table 4 show that the anisotropic field strength H a and the permeability ⁇ can be adjusted in a targeted manner by adjusting the tension o a .
  • M is one or more of Mo, Ta, or Zr with 0 ⁇ b + c ⁇ 2,
  • T is one or more of the elements V, Mn, Cr, Co or Ni with 0 ⁇ d ⁇ 5, Si 10 ⁇ x ⁇ 18
  • Z is one or more of the elements C, P or Ge with 0 ⁇ z ⁇ 2, wherein the alloy can have up to 1 atom% of impurities.
  • Typical impurities are C, P, S, Ti, Mn, Cr, Mo, Ni, and Ta.
  • the composition can exert an influence on the magnetic properties in certain heat treatments.
  • the heat treatment and in particular the tensile stress can be adjusted.
  • Table 5 shows examples of the alloy, which were approximately 4 seconds heat-treated under a tension of 50 MPa at an optimum for the respective composition tempering temperature T A, and a Comparative Example having a composition with a niobium content of above 2 atomic%.
  • the remaining examples, numbered 1 to 10, represent compositions according to the invention having an Nb content of less than 2 at%.
  • FIG. 10 additionally shows the optimum tempering temperatures and the crystallization temperatures of alloy examples 1 to 10.
  • FIG. 10 shows the lower and upper optimum Tempering temperature T al and T a2 for a tempering time of 4 s as a function of the crystallization temperatures T xl and T x2 measured in the DSC at 10 K / min.
  • alloys according to the invention can be varied within certain limits.
  • limits (1) instead of Nb further elements such as Mo, Ta and / or Zr (2) instead of iron other transition metals such as V, Mn, Cr, Co and or Ni or (3) elements such as C, P and / or Ge can be added without the properties change significantly.
  • the alloy composition was used as another embodiment
  • Table 6 therefore shows other examples of alloys in which the Cu content was varied systematically and a heat treatment of about 7 seconds duration was carried out at 600 ° C under a tensile stress of about 15 MPa.
  • the element Fe was gradually replaced by Cu, with the remaining alloying components remaining unchanged.
  • Table 6 shows no significant influence of the Cu content on the magnetic properties for Cu contents below 1.5at%.
  • the addition of Cu promotes the Embrittlement tendency of the strips during production.
  • alloys with Cu contents greater than 1.5at% (such as, for example, alloy no. 15 from Table 6) already exhibit a strong embrittlement in the production state, so that a 20 ⁇ m thick band of the alloy Fe 74.5 Cu 2 1.5 Si 15.5 B 6.5 in a Bending diameter of about 1 mm can break.
  • Such a brittle belt can not be caught or wound up directly during the casting process due to the high production line speeds (25-30 m / s) after leaving the cooling roller or only with great difficulty during the casting process. This makes the tape production uneconomical. Also, such break even at the beginning of brittle bands in the heat treatment to an increased extent, especially before they enter the zone of elevated temperature. With such a break, the heat treatment process is interrupted and the tape must be threaded through the oven again.
  • alloys with a Cu content of less than 1.5at% can be bent to a bending diameter of twice the strip thickness, ie typically less than 0.06 mm, without breaking. This allows the tape to be rewound directly during casting. Furthermore, the heat treatment of such initially ductile bands is much easier. Alloys with a Cu content of less than 1.5 at% become embrittled only after the heat treatment, but only after they have left the furnace and are cooled again. The probability of a ligament tear during the heat treatment is thus significantly lower. Also, in most cases, belt transport through the oven can continue despite demolition. All in all, ductile tapes can thus be produced more easily and thus more economically, as well as heat-treated at first.
  • the compositions shown in Tables 5 and 6 are nominal compositions in at% which coincide, within an accuracy of typically +0.5 at%, with the concentrations of the individual elements found in the chemical analysis.
  • the silicon content and the boron content also exert an influence on the magnetic properties of this type of nanocrystalline alloy with a niobium content of less than 2 atomic% when it is produced under tensile stress.
  • FIG. 11 shows a diagram of the course of coercive field strength H c and remanence ratio J r / ' J s of both alloys after heat treatment under a tensile stress of about 50 MPa as a function of tempering temperature T a .
  • the coercive field strength H c and the remanence ratio J r / J s of the alloy Fe 80 S 11B 9 according to the invention are represented by filled circle symbols and the comparative composition Fe 78 . 5 SiioBii.5 shown by open triangular symbols, after a heat treatment of 4 seconds duration at the tempering temperature T a under a tensile stress of about 50 MPa.
  • FIG. 12 shows a diagram of hysteresis loops of the two alloys after heat treatment for 4 s at about 565 ° C. under tensile stresses of 50 MPa (dashed line) or 220 MPa (solid line).
  • the hysteresis loop of the alloy according to the invention Fe 8 OSinB 9 is on the left and that of the comparative composition Fe 7 8.5 SiioBii. 5 is shown on the right.
  • the inventive composition Fe 8o SINB 9 after heat treatment between about 530 ° C and 570 ° C, a linear magnetization loop with a small remanence J r / J s ⁇ 0.1 and a low coercive field strength onto which is clearly below 100 A / m and finally only a few percent of the anisotropic field strength H a .
  • the composition Fevs.siioBn.s has a high remanence ratio throughout the entire heat treatment range.
  • the upper limit of the Si content and the lower limit of the boron content are also examined. While the alloy composition Fe75Cuo.5Nb1.5Si17.5B5.5 (see alloy no. 5 of Table 5) was produced as an amorphous, ductile band easily and had to heat treatment desirable properties, the alloy composition Fe had 7 5Cuo.5 bi.5Sii 8 B 5 after heat treatment only borderline magnetic properties and the alloy composition Fe 75 Cu o.5 bi .5 Sii 8.5 B 4.5 could no longer be prepared as a ductile amorphous band.
  • Table 7 shows the saturation magnetostriction constant ⁇ ⁇ of various alloy compositions measured in the state of manufacture and after 4s heat treatment under a tension of 50 MPa at the indicated tempering temperature T a .
  • an annealing temperature was chosen, which is distant from the maximum annealing temperature T a2 not more than 50 ° C, as this particularly small for a given composition values of the magnetostriction are obtained (see Figure 5) which will ultimately be determined by the alloy composition.
  • the effect of the Si content of the alloy is shown.
  • Table 7 demonstrates that, after heat treatment under tensile stress, a significant reduction in the saturation magnetostriction results, which can lead to reproducible magnetic properties.
  • a small amount of magnetostriction is the more important the higher the permeability.
  • alloys with a permeability greater than 500 or greater than 1000 have a comparatively low dependence on mechanical stresses if the saturation magnetostriction is less than 2 ppm or less than 1 ppm.
  • the alloy may also have a saturation magnetostriction of less than 5 ppm in magnitude. Alloys with a saturation magnetostriction below these limits still have good soft magnetic properties even at internal stress, when the permeability is less than 500.
  • the value of the saturation magnetostriction may still slightly depend on the tensile stress o a applied during the heat treatment.
  • the result is alloy
  • the apparatus 1 has a continuous furnace 2 with a temperature zone 3, this temperature zone being set so that the temperature in the furnace in this zone is within 5 ° C. of the tempering temperature T a .
  • the device 1 further comprises a coil 4, on which the amorphous alloy 5 is wound, and a take-up spool 6, on which the heat-treated belt 7 is received.
  • the tape is drawn at a speed s from the spool 4, through the continuous oven 2 to the take-up spool 6.
  • the belt 7 is in the direction of the device 9 to the device 10 under a tensile stress ⁇ .
  • the apparatus 1 further comprises an apparatus 8 for continuously measuring the magnetic properties of the belt 6 after it has been heat treated and drawn out of the continuous furnace 2.
  • the belt 7 is no longer under tension.
  • the measured magnetic properties can be used to set the tension under which the belt 7 is pulled through the continuous furnace 2. This is schematically illustrated by the arrows 9 and 10 in FIG.

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Abstract

L'invention concerne un alliage qui est constitué de Fe100-a-b-c-d-x-y-zCuaNbbMcTdSixByZz et jusqu'à 1 % atomique d'impuretés, M étant un ou plusieurs des éléments Mo, Ta ou Zr, T un ou plusieurs des éléments V, Mn, Cr, Co ou Ni et Z un ou plusieurs des éléments C, P ou Ge et 0 % atom ≤ a < 1,5 % atomique, 0 % atom ≤ b < 2 % atom, 0 % atom ≤ (b+c) < 2 % atom, 0 % atom ≤ d < 5 % atom, 10 % atom < x < 18 % atom, 5 % atom < y < 11 % atom et 0 % atom ≤ z < 2 % atom. L'alliage est configuré en forme de bande et présente une structure nanocristalline dans laquelle au moins 50 % en volume des grains présentent une grosseur moyenne inférieure à 10 nm, un cycle d'hystérésis avec une partie linéaire centrale, un rapport de rémanence, Jr/Js, < 0,1 et un rapport de la force de champ coercitif, Hc, à la force de champ anisotrope, Ha, < 10 %.
EP12720963.3A 2011-04-15 2012-04-05 Alliage, noyau magnétique et procédé pour fabriquer une bande d'un alliage Active EP2697399B1 (fr)

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DE102011002114A DE102011002114A1 (de) 2011-04-15 2011-04-15 Legierung, Magnetkern und Verfahren zum Herstellen eines Bandes aus einer Legierung
PCT/IB2012/051682 WO2012140550A1 (fr) 2011-04-15 2012-04-05 Alliage, noyau magnétique et procédé pour fabriquer une bande d'un alliage

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WO2014126220A1 (fr) * 2013-02-15 2014-08-21 日立金属株式会社 Noyau magnétique annulaire utilisant un alliage magnétique doux nanocristallin à base de fer et constituant magnétique utilisant ledit noyau magnétique annulaire
KR20150143251A (ko) * 2014-06-13 2015-12-23 삼성전기주식회사 코어 및 이를 갖는 코일 부품
WO2016005932A1 (fr) * 2014-07-10 2016-01-14 Colognesi Ernesto Dispositif et procédé permettant la production et le transfert d'une énergie de chauffage et de refroidissement
US11264156B2 (en) * 2015-01-07 2022-03-01 Metglas, Inc. Magnetic core based on a nanocrystalline magnetic alloy
US11230754B2 (en) 2015-01-07 2022-01-25 Metglas, Inc. Nanocrystalline magnetic alloy and method of heat-treatment thereof
JP6226093B1 (ja) * 2017-01-30 2017-11-08 Tdk株式会社 軟磁性合金および磁性部品
DE112018003444T5 (de) * 2017-07-04 2020-04-16 Hitachi Metals, Ltd. Band aus amorpher Legierung und Verfahren zur Herstellung desselben
DE102019105215A1 (de) * 2019-03-01 2020-09-03 Vacuumschmelze Gmbh & Co. Kg Legierung und Verfahren zur Herstellung eines Magnetkerns
DE102019123500A1 (de) * 2019-09-03 2021-03-04 Vacuumschmelze Gmbh & Co. Kg Metallband, Verfahren zum Herstellen eines amorphen Metallbands und Verfahren zum Herstellen eines nanokristallinen Metallbands

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DE102011002114A1 (de) 2012-10-18
WO2012140550A1 (fr) 2012-10-18
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EP2697399B1 (fr) 2015-03-25
KR20140014188A (ko) 2014-02-05
CN103502481B (zh) 2016-02-17
DE102011002114A9 (de) 2013-01-17
JP2014516386A (ja) 2014-07-10
JP6040429B2 (ja) 2016-12-07

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