EP2416329B1 - Magnetic core for low-frequency applications and manufacturing process of a magnetic core for low-frequency applications - Google Patents
Magnetic core for low-frequency applications and manufacturing process of a magnetic core for low-frequency applications Download PDFInfo
- Publication number
- EP2416329B1 EP2416329B1 EP10172135.5A EP10172135A EP2416329B1 EP 2416329 B1 EP2416329 B1 EP 2416329B1 EP 10172135 A EP10172135 A EP 10172135A EP 2416329 B1 EP2416329 B1 EP 2416329B1
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- European Patent Office
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- magnetic core
- tape
- heat treatment
- temperature
- coating
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Images
Classifications
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- 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)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- 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
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
-
- 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
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- 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
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- 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
-
- 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
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- 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
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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- 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
- H01F1/14766—Fe-Si based alloys
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/25—Magnetic cores made from strips or ribbons
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F3/00—Cores, Yokes, or armatures
- H01F3/04—Cores, Yokes, or armatures made from strips or ribbons
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- 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
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49002—Electrical device making
- Y10T29/4902—Electromagnet, transformer or inductor
Definitions
- the invention relates to a magnetic core for low-frequency applications from a spirally wound, soft magnetic, nanocrystalline tape, which should be suitable in particular for use in residual current circuit breakers (FI-switches).
- FI-switches residual current circuit breakers
- Residual current circuit breakers are used to protect people and equipment against electric shock.
- the energy required to operate the release triggering the cut-out must be provided solely by the fault current.
- Protective currents of 300 mA, 500 mA or 1000 mA are typical for device protection.
- the tripping current must not exceed 30 mA.
- Special personal protection switches even have triggering thresholds of 10 mA.
- the switches must work properly in the range between -5 ° C and 80 ° C. For switches with increased requirements, the working range is between -25 ° C and 100 ° C.
- AC-sensitive RCCBs must have the required sensitivity for sinusoidal fault currents. They must reliably trigger both sudden and slowly increasing fault currents, which places certain demands on the eddy current behavior of the material.
- the residual current transformer is bipolar controlled. in the Falling residual current must at least be sufficient for its secondary voltage in order to trigger the magnet system of the release.
- a material is required which has the highest possible permeability at the operating frequency of typically 50 Hz.
- pulse current-sensitive RCD switches must reliably trip even with single or full wave rectified currents with and without phase control and with superimposed DC component, regardless of the current direction. Because of the high remanence induction, round loop converters have only a small unipolar induction swing, which may make the delivered trip voltage too small for pulsed fault currents. This leads to the increased use of flat-core transducer cores which, while having a high unipolar induction stroke, have significantly lower permeabilities than those with a circular loop.
- the tripping power to be applied by the converter core should be as high as possible.
- the main influencing factors here are the geometry of the core and the magnetic material properties in combination with the technological refinement of the material, for example by a heat treatment.
- NiFe alloys made of NiFe alloys.
- the high-permeability 75-80% NiFe materials also called “ ⁇ -metal” or “permalloy” with a round or flat loop were particularly well suited for sensitive personal protection switches. These materials have a saturation induction of about 0.8 T and achieve maximum permeabilities of 300,000 and more.
- the dynamic properties for transmitting harmonic content in non-sinusoidal fault currents are not ideal.
- causes are the relatively high band thicknesses of 50 to 150 microns and the relatively low resistivity of 0.5 ⁇ m ⁇ ⁇ ⁇ 0.6 microns.
- the setting of a corresponding behavior of the temperature coefficient requires a cost-consuming effort in the heat treatment.
- the magnetization process of Z loops is based on wall displacement processes whose activation requires a minimum field strength dependent on the respective material, the small signal permeability, in particular the initial permeability, such as ⁇ 1 , is particularly low there.
- the frequency response of the permeability and the behavior in fast magnetization processes are not optimal, since due to pronounced eddy current anomalies takes place already in the low frequency range, a strong decrease in permeability.
- such cores are not well suited for small fault current signals.
- Such magnetic cores are usually subjected to a heat treatment in the magnetic field. If these are to be operated economically, the nuclei for the heat treatment are too pile. Due to the spatial dependence of the demagnetization factor of a cylinder, the stacked nuclei experience a magnetization that is spatially dependent in the axial direction, even in weak stray fields such as the Earth's field. This leads to strong location-dependent scattering of the magnetic properties in the necessarily very small magnetic field-induced anisotropies for the application under consideration. These manifest themselves, for example, in permeability dispersions, which make considerable sorting and finishing work necessary in manufacturing practice. In addition, the dead weight of the stacked cores leads to a superimposed asymmetric magnetomechanically induced gear of the magnet values along the stack.
- the starting material of these alloys is produced by melt spinning technology as a first amorphous band.
- the wound toroidal cores are subjected to a heat treatment in which the amorphous state turns into a nanocrystalline two-phase structure with excellent soft magnetic properties.
- An important prerequisite for the industrial realization of highest permeability values over a wide field strength range from 1 mA / cm to over 50 mA / cm is a minimization of the magnetostriction (saturation magnetostriction) to values
- the alloy spectrum is limited, on the other hand, in the heat treatment, the crystallization temperature for the generation and maturation of the nanorod is alloy-specifically adapted so that the volume fraction of the nanocrystalline phase with low, occasionally even negative magnetostriction is formed so strong that the high positive magnetostriction of the amorphous residual phase compensated as best as possible.
- a magnetic core for low frequency applications is provided from a spirally wound, soft magnetic, nanocrystalline ribbon, wherein the ribbon is substantially the alloy composition Fe remainder CO a cub c s d B e C f wherein a, b, c, d, e and f are in atomic percent and 0 ⁇ a ⁇ 1; 0.7 ⁇ b ⁇ 1.4; 2.5 ⁇ c ⁇ 3.5; 14.5 ⁇ d ⁇ 16.5; 5.5 ⁇ e ⁇ 8 and 0 ⁇ f ⁇ 1 and cobalt may be wholly or partially replaced by nickel, wherein the magnetic core has a saturation magnetostriction ⁇ s with
- the band has a band thickness d with d ⁇ 24 ⁇ m, preferably d ⁇ 21 ⁇ m and an effective roughness depth R a (eff) with R a (eff) ⁇ 7%, preferably R a (eff) ⁇ 5%.
- a strip which essentially has a certain alloy composition is understood here and below to mean a strip whose alloy is additionally embedded in the strip low concentrations may contain impurities typical of other elements.
- a sealing coating arranged on the strip surfaces is understood here and below as meaning a coating which tightly seals the predominant parts or even the entire strip surface.
- the magnetostriction of such alloys can be adjusted to zero as far as possible with a suitable heat treatment.
- the magnet values are insensitive to mechanical influences, which allows a wide range of core shapes and fixations.
- the temperature characteristic of the permeability may become negative, which may be advantageous in various embodiments of FI switches.
- the heat treatment is advantageously carried out in such a way that the local magnetostriction contributions of the nanorod and of the amorphous residual phase balance as best as possible.
- the strip surfaces at the required temperatures of more than 540 ° C have a clear tendency to crystalline precipitates.
- these may consist of the known FeB 2 phases or of macrocrystalline precipitates such as Fe 2 O 3 , Fe 3 O 4 and Nb 2 O 5 .
- Their formation is favored by the roughness of the strip surfaces, an increased strip thickness, too low a metalloid content, but also by metal-gas reactions between impurities in the protective gas and the strip surface.
- the formation of oxidic surface layers, for example of SiO 2 plays an important role. The resulting with such surface effects anisotropies and crystal lead to increased field strengths, low remanence values and reduced permeability values.
- the formation of crystalline precipitates can be avoided by the sealing coating.
- the strip has a strip thickness d with d ⁇ 24 ⁇ m, preferably d ⁇ 21 ⁇ m.
- the band has an effective surface roughness R a (eff) with R a (eff) ⁇ 7%, preferably R a (eff) ⁇ 5%.
- the effective roughness depth is determined in practice, for example by means of the Rugotest or the Tastroughmethode.
- the tape has a total metal content c + d + e + f> 22.5 at%, preferably c + d + e + f> 23.5 at%.
- the oxide coating contains magnesia. According to a further embodiment, the oxide coating contains zirconium oxide. Alternatively or additionally, the oxide coating may contain oxides of an element selected from the group consisting of Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, further elements of main groups 2 and 3 and the group of rare earth metals.
- Such coating of the strip before the heat treatment makes it possible to carry out the heat treatment at the relatively high temperature necessary for the adjustment of the magnetostriction without sacrificing crystalline precipitates and / or vitreous layers of SiO 2 and, associated therewith, deterioration of the magnet values to have to take.
- This procedure allows the production of magnetic cores having a maximum permeability ⁇ max with ⁇ max > 500,000, preferably ⁇ max > 600,000, and an initial permeability ⁇ 1 of ⁇ 1 > 150,000, preferably ⁇ 1 > 200,000, the magnetic core having a remanence ratio B R / B S with B R / B S > 70%.
- the saturation magnetostriction ⁇ s can be reduced to
- the finished magnetic core is no longer very sensitive to tension. It can then be fixed in a protective trough, for example, with a pressure-sensitive adhesive and / or with a ring of an elastic material placed on top of one or both ends of the magnetic core.
- a pressure-sensitive adhesive for example, silicone rubber, acrylate or silicone grease can be used as adhesives.
- the magnetic core may have an epoxy vertebral interlayer on one or both end faces.
- such a magnetic core is used in a residual current circuit breaker.
- a method of manufacturing a magnetic core for low frequency applications from a spirally wound, soft magnetic, nanocrystalline tape wherein the tape is substantially the alloy composition Fe remainder CO a Cu b Nb c Si d B e C f wherein a, b, c, d, e and f are in atomic percent and 0 ⁇ a ⁇ 1; 0.7 ⁇ b ⁇ 1.4; 2.5 ⁇ c ⁇ 3.5; 14.5 d ⁇ 16.5; 5.5 ⁇ e ⁇ 8 and 0 ⁇ f ⁇ 1 and cobalt may be wholly or partially replaced by nickel.
- the tape is provided with a coating of a metal alkoxide solution and / or an acetyl-acetone chelate complex with a metal from which forms a sealing coating of a metal oxide in a subsequent heat treatment for nanocrystallization of the tape.
- ⁇ 2 ppm preferably
- the heat treatment is carried out in an inert gas atmosphere of H 2 , N 2 and / or Ar, wherein the dew point T P ⁇ -25 ° C or the dew point T P ⁇ -49, 5 ° C.
- the metal for the coating advantageously an element selected from the group Mg, Zr, Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, other elements of the 2nd and 3rd main group and the group of rare earth metals be used.
- the unstacked magnetic cores are placed on a good thermal conductivity carrier during the continuous annealing process.
- a good thermal conductivity carrier consists for example of a good heat-conducting metal such as copper, silver or good heat-conducting steel.
- the carrier is also a bed of good thermal conductivity ceramic powder.
- the toroidal cores can be set on the face side to copper plates with a thickness of at least 4mm, preferably at least 6mm, more preferably at least 10mm. This helps to avoid local overheating when the exothermic crystallization sets in, in which the released heat of crystallization is effectively dissipated.
- the persistence in the decay zone serves to decay the heat of crystallization before further heating of the magnetic core to avoid local overheating.
- the heat treatment is carried out in an inert gas atmosphere of H 2 , N 2 and / or Ar, wherein the dew point T P ⁇ -25 ° C, preferably T P ⁇ -49.5 ° C.
- the strip is wound with decreasing strip tension to the magnetic core.
- FIG. 1 schematically shows an AC-sensitive FI switch 1, which separates the monitored circuit all poles of the rest of the network when a certain differential current is exceeded.
- the comparison of the currents flowing through the FI-switch 1 takes place in a summation current transformer 2, by which the currents flowing to and from the load are added with the correct sign. If a current is dissipated in the circuit to ground, then in the summation current transformer, the sum of back and forth flowing current is not equal to zero: there is a difference in current, which leads to the response of the residual current circuit breaker 1 and thus to the shutdown of the power supply.
- the summation current transformer 2 has a magnetic core 2, which is wound from a nanocrystalline soft magnetic strip.
- the FI-switch 1 further includes a trigger relay 4, a biased latch 5 and a test button 6 for manually checking the FI-switch. 1
- FIG. 2 schematically shows a possible temperature profile of a heat treatment according to a method for producing a magnetic core according to an embodiment of the invention.
- the temperature in the ripening zone is adapted to the composition of the respective batch so that the magnitude of the magnetostriction value becomes minimal.
- preliminary samples are first prepared of the strip batches to be used which are exposed to different temperatures T x between 540 ° C. and 600 ° C. in the ripening zone.
- the subsequent determination of the magnetostriction is carried out either directly on a removed piece of tape or indirectly on an undamaged core.
- the direct measurement can be done for example by means of the SAMR method.
- An indirect method is a pressure test in which the circumference of the toroidal core is deformed for example by 2% to the oval.
- the occurring change in the coercive field strength is determined by measuring the quasi-static hysteresis loop by means of a remainder graph before and during the deformation.
- FIG. 4 gives the lot-specific optimal value for T x can be read where the change ⁇ H c is minimal or even goes to zero.
- Suitable substances are dissolved substances whose starting materials sinter during the annealing process in an H 2 , N 2 or Ar protective gas atmosphere or mixtures thereof at temperatures up to 650 ° C. to form an oxidic, thermally stable layer and are not reduced by the action of the protective gases.
- base materials of such coatings are Be, Mg, Al, Zr, Ti, V, Nb, Ta, Ce, Nd, Gd and other elements of the 2nd and 3rd main groups and the group of SE elements. These are used as metal alkoxide solutions in the respective corresponding alcohol or ether, for example methylate, ethylate, propylate or butylate solutions in the corresponding alcohol or dissolved in ether alkylates or, for example, as tri- or tetra-Isopropylalkoholate applied to the tape surfaces.
- Other alternatives include acetyl-acetone chelate complexes with the metals mentioned.
- Typical layer thicknesses are in the range of 0.05 to 5 .mu.m, with a layer thickness in the range of 0.2 to 1 .mu.m having sufficiently good properties and therefore being preferred in one embodiment.
- the coating makes it possible to stabilize the material properties at the high temperatures necessary for the zero adjustment of the magnetostriction against surface reactions.
- the application-relevant parameters influenced by surface effects are, in particular, the ⁇ (H) characteristic curve measured at 50 Hz, the quasi-static coercive field strength and the remanence induction.
- the layer thicknesses mentioned can each be achieved by adjusting the concentration and by adapting the process parameters. If particularly thick layers are to be achieved, the process can also be repeated.
- the belt is in a continuous process via pulleys running through the located in a tub Drawn coating medium. Immediately before winding to the core, it passes through a drying section controlled at 80-200 ° C. This process is characterized by a special uniformity of the coating. Repeated cycles allow thicker layers to be achieved.
- the wound after production tape is dipped as a coil in the standing in a recipient solution and evacuated. Due to the capillary forces which are sufficiently effective at a vacuum in the region of the rough vacuum of 10-300 mbar, the solution penetrates between the band layers of the coil and wets the surfaces. The dried coils are subsequently dried in a drying oven at 80-200 ° C. The coated tape is then wound into magnetic cores. This process is particularly economical.
- the cores wound from uncoated tape are immersed in a recipient in the solution. After evacuation to the above negative pressure, the solution penetrates between the tape layers and wets them. The submerged cores are then dried at 80 to 200 ° C in a drying oven. This method has the advantage that the winding process of the core can not be disturbed by the coating medium on the strip surfaces.
- the concentration of the dissolved metals was varied in the various organic solvents in a wide range between 0.1% by weight and 5% by weight without significant changes in the magnetic values. However, at very low concentrations, there was an increase in scattering.
- both the coated and the uncoated strips were wound with decreasing strip tension to tension-free ring band cores of the dimension 32 mm by 16 mm by 10 mm.
- 100 cores were placed on the face side on square copper plates measuring 300 mm by 300 mm by 6 mm.
- the subsequent heat treatment was completely field-free in a continuous process with a temperature profile similar to in FIG. 2 shown, wherein the passage speed through the heating zone was 0.16 m / min.
- the protective gas was pure hydrogen with a dew point of -50 ° C. in the Contrary to the representation in FIG. 2 the temperature gradient was increased in the first heating zone such that the annealing material reached a temperature of 480 ° C after only 8 minutes.
- the temperature in the decay zone was not kept constant, but increased from 480 ° C to 505 ° C along a 20-minute heating. This was followed by a steep temperature gradient, which the cores passed through within 3 minutes to reach the final maturation temperature T x . This temperature range was completed within 25 minutes.
- the cores were used at the same throughput speed in contrast to FIG. 2 significantly extended cooling zone cooled for one hour under hydrogen the same dew point to room temperature. This greatly delayed cooling rate was chosen to avoid cooling-induced stress effects.
- the remanence ratio B R / B S was 77%.
- the dew point was varied between -20 ° C and -55 ° C by mixing humidified and dry H 2 gas. To measure the dew point the device PANAMETRICS MIS1 was used.
- the test cores were annealed with the same temperature profile on copper plates, as already mentioned above in addition to FIG. 2 has been described.
- all cores proved to be magnetostrictive during a deformation test and therefore could not be further processed with the usual one-trough method for magnetostriction-free cores. Rather, special non-spanning one-trough procedures were necessary.
- the ⁇ 1 values at 50 Hz were measured at the cores and in FIG. 14 applied over the effective surface roughness. As in FIG. 14 is recognizable, an effective surface roughness of R 3 (eff) ⁇ 7% is required to realize ⁇ 1 ⁇ 100,000. If ⁇ 1 is greater than 160,000, R a (eff) should be less than 5%, for ⁇ 1 greater than 200,000, even less than 2.5%.
- the cores could be glued into a plastic trough by means of silicone rubber or loosely inserted into a plastic or metal protective trough by means of a mechanically dampening foam rubber ring, without any appreciable change in permeability.
- the results of the investigations are summarized in Table 1.
- the marking *) means a fixation with silicone rubber and the marking **) a non-tensioning fixation with a high-viscosity acrylate adhesive.
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Description
Die Erfindung betrifft einen Magnetkern für Niederfrequenzanwendungen aus einem spiralförmig aufgewickelten, weichmagnetischen, nanokristallinen Band, der insbesondere für den Einsatz in Fehlerstromschutzschaltern (FI-Schaltern) geeignet sein soll.The invention relates to a magnetic core for low-frequency applications from a spirally wound, soft magnetic, nanocrystalline tape, which should be suitable in particular for use in residual current circuit breakers (FI-switches).
Fehlerstromschutzschalter dienen dem Schutz von Personen und Einrichtungen gegen elektrischen Stromschlag. Entsprechend der Norm DIN EN 61008/DIN VDE 0664 muss die Energie zur Betätigung des Auslösers, der die Abschaltung hervorruft, ausschließlich durch den Fehlerstrom geliefert werden. Für den Geräteschutz sind Auslöseströme von 300 mA, 500 mA oder 1000 mA typisch. Für den Personenschutz darf der Auslösestrom dagegen 30 mA nicht überschreiten. Spezielle Personenschutzschalter besitzen sogar Auslöseschwellen von 10 mA. Nach der Norm müssen die Schalter im Bereich zwischen -5°C und 80°C einwandfrei arbeiten. Bei Schaltern mit erhöhten Anforderungen liegt der Arbeitsbereich zwischen -25°C und 100°C.Residual current circuit breakers are used to protect people and equipment against electric shock. In accordance with the standard DIN EN 61008 / DIN VDE 0664, the energy required to operate the release triggering the cut-out must be provided solely by the fault current. Protective currents of 300 mA, 500 mA or 1000 mA are typical for device protection. For personal protection, however, the tripping current must not exceed 30 mA. Special personal protection switches even have triggering thresholds of 10 mA. According to the standard, the switches must work properly in the range between -5 ° C and 80 ° C. For switches with increased requirements, the working range is between -25 ° C and 100 ° C.
Man unterscheidet wechselstromsensitive und pulsstromsensitive FI-Schalter.A distinction is made between AC-sensitive and pulse-current-sensitive FI switches.
Wechselstromsensitive FI-Schalter müssen die geforderte Empfindlichkeit bei sinusförmigen Fehlerströmen aufweisen. Sie müssen sowohl bei plötzlich als auch bei langsam ansteigenden Fehlerströmen zuverlässig auslösen, was gewisse Anforderungen an das Wirbelstromverhalten des Materials stellt. In diesem Fall wird der Fehlerstromwandler bipolar ausgesteuert. Im Fehlerstromfall muss dessen Sekundärspannung zumindest ausreichen, um das Magnetsystem des Auslösers auszulösen. Für eine platzsparende Auslegung des Wandlerkerns wird ein Material benötigt, das bei der Arbeitsfrequenz von typischerweise 50 Hz eine möglichst hohe Permeabilität aufweist. Da mit der R-Schleife (runde Form der Hystereseschleife) sowohl im Bereich der Anfangspermeabilität als auch bei der Feldstärke der Maximalpermeabilität sehr hohe 50Hz-Permeabilitätswerte realisierbar sind, hat sich diese weitgehend für ausschließlich wechselstromsensitive FI-Schalter durchgesetzt. Der optimale Arbeitspunkt liegt dabei im Bereich der Maximalpermeabilität oder etwas darüber.AC-sensitive RCCBs must have the required sensitivity for sinusoidal fault currents. They must reliably trigger both sudden and slowly increasing fault currents, which places certain demands on the eddy current behavior of the material. In this case, the residual current transformer is bipolar controlled. in the Falling residual current must at least be sufficient for its secondary voltage in order to trigger the magnet system of the release. For a space-saving design of the converter core, a material is required which has the highest possible permeability at the operating frequency of typically 50 Hz. Since with the R-loop (round shape of the hysteresis loop) very high 50 Hz permeability values can be realized both in the area of the initial permeability and in the field strength of the maximum permeability, this has largely prevailed for exclusively AC-sensitive FI switches. The optimal operating point is in the range of the maximum permeability or something above it.
Pulsstromsensitive FI-Schalter müssen darüber hinaus auch bei ein- oder zweiweggleichgerichteten Strömen mit und ohne Phasenanschnitt und mit überlagertem Gleichstromanteil unabhängig von der Stromrichtung zuverlässig auslösen. Wegen der hohen Remanenzinduktion besitzen Wandler mit runder Schleife nur einen kleinen unipolaren Induktionshub, wodurch die gelieferte Auslösespannung bei pulsförmigen Fehlerströmen zu klein sein kann. Dies führt zum vermehrten Einsatz von Wandlerkernen mit flacher Schleife, die zwar einen hohen unipolaren Induktionshub, aber gleichzeitig deutlich niedrigere Permeabilitäten als solche mit runder Schleife besitzen.In addition, pulse current-sensitive RCD switches must reliably trip even with single or full wave rectified currents with and without phase control and with superimposed DC component, regardless of the current direction. Because of the high remanence induction, round loop converters have only a small unipolar induction swing, which may make the delivered trip voltage too small for pulsed fault currents. This leads to the increased use of flat-core transducer cores which, while having a high unipolar induction stroke, have significantly lower permeabilities than those with a circular loop.
Um im geforderten Fehlerstrombereich ein zuverlässiges Auslöseverhalten zu erzielen, sollte die vom Wandlerkern aufzubringende Auslöseleistung möglichst hoch sein. Die wesentlichen Einflussfaktoren sind hierfür die Geometrie des Kerns sowie die magnetischen Werkstoffeigenschaften in Kombination mit der technologischen Veredelung des Materials beispielsweise durch eine Wärmebehandlung.In order to achieve a reliable tripping behavior in the required fault current range, the tripping power to be applied by the converter core should be as high as possible. The main influencing factors here are the geometry of the core and the magnetic material properties in combination with the technological refinement of the material, for example by a heat treatment.
Einzelheiten zu Wandlerwerkstoffen für wechselstrom- und pulsstromsensitive FI-Schalter sind in verschiedenen Veröffentlichungen dargelegt, beispielsweise in
In früheren Jahren kamen fast ausschließlich Summenstromwandler aus NiFe-Legierungen zum Einsatz. Dabei eigneten sich die hochpermeablen 75-80prozentigen NiFe-Werkstoffe (auch "µ-Metall" oder "Permalloy" genannt) mit runder oder flacher Schleife besonders gut für empfindliche Personenschutzschalter. Diese Werkstoffe besitzen eine Sättigungsinduktion von ca. 0,8 T und erreichen Maximalpermeabilitäten von 300.000 und mehr. Allerdings sind die dynamischen Eigenschaften zur Übertragung des Oberwellenanteils bei nichtsinusförmigen Fehlerströmen nicht ideal. Ursachen sind die relativ hohen Banddicken von 50 bis 150 µm und der relativ niedrige spezifische Widerstand von 0,5 µΩm ≤ ρ ≤ 0,6 µm. Außerdem benötigt die Einstellung eines entsprechenden Verhaltens des Temperaturkoeffizienten einen kostentreibenden Aufwand bei der Wärmebehandlung.In previous years almost exclusively summation current transformers made of NiFe alloys were used. The high-permeability 75-80% NiFe materials (also called "μ-metal" or "permalloy") with a round or flat loop were particularly well suited for sensitive personal protection switches. These materials have a saturation induction of about 0.8 T and achieve maximum permeabilities of 300,000 and more. However, the dynamic properties for transmitting harmonic content in non-sinusoidal fault currents are not ideal. Causes are the relatively high band thicknesses of 50 to 150 microns and the relatively low resistivity of 0.5 μΩm ≤ ρ ≤ 0.6 microns. In addition, the setting of a corresponding behavior of the temperature coefficient requires a cost-consuming effort in the heat treatment.
Seit Kurzem haben sich in pulsstromsensitiven FI-Schaltern auch nanokristalline FeCuNbSiB-Werkstoffe durchgesetzt. Wichtige Vorteile sind die hohe Sättigungsinduktion von ca. 1,2 T, die hervorragende Linearität der F-Schleife (flache Hystereseschleife) von µ4/µ15 = 0,65-0,95 bei einem weiträumig einstellbaren µ-Niveau von mehr als 100.000. Daneben weisen diese Werkstoffe hervorragende dynamische Eigenschaften auf, die sich auf eine geringe Banddicke von 15-30 µm und einen vergleichsweise hohen spezifischen Widerstand von 1,1 µΩm ≤ ρ ≤ 1,3 µΩm zurückführen lassen. Auf derartige Werkstoffe bezieht sich die
Für wechselstromsensitive Wandlerkerne mit R-Schleife aus nanokristallinen Legierungen offenbart die
Derartige Magnetkerne werden meist einer Wärmebehandlung im Magnetfeld unterzogen. Soll diese in wirtschaftlicher Weise betrieben werden, sind die Kerne für die Wärmebehandlung zu stapeln. Aufgrund der Ortsabhängigkeit des Entmagnetisierungsfaktors eines Zylinders erfahren die gestapelten Kerne auch in schwachen Streufeldern wie dem Erdfeld eine in axia-ler Richtung ortsabhängige Magnetisierung. Diese führt bei den für die betrachtete Anwendung notwendigerweise sehr kleinen magnetfeldinduzierten Anisotropien zu starken ortsabhängigen Streuungen der magnetischen Eigenschaften. Diese manifestieren sich beispielsweise in Permeabilitätsstreuungen, die in der Fertigungspraxis erheblichen Sortier- und Nachbearbeitungsaufwand erforderlich machen. Darüber hinaus führt das Eigengewicht der gestapelten Kerne zu einem überlagerten unsymmetrischen, magnetomechanisch induzierten Gang der Magnetwerte entlang des Stapels.Such magnetic cores are usually subjected to a heat treatment in the magnetic field. If these are to be operated economically, the nuclei for the heat treatment are too pile. Due to the spatial dependence of the demagnetization factor of a cylinder, the stacked nuclei experience a magnetization that is spatially dependent in the axial direction, even in weak stray fields such as the Earth's field. This leads to strong location-dependent scattering of the magnetic properties in the necessarily very small magnetic field-induced anisotropies for the application under consideration. These manifest themselves, for example, in permeability dispersions, which make considerable sorting and finishing work necessary in manufacturing practice. In addition, the dead weight of the stacked cores leads to a superimposed asymmetric magnetomechanically induced gear of the magnet values along the stack.
Zur Umgehung dieser Probleme wird in der
Für Magnetkerne für Hochfrequenzanwendungen werden seit Langem Isolationsbeschichtungen zwischen den Bandlagen zur Verminderung von Wirbelströmen eingesetzt. Dies ist beispielsweise aus der
Aufgabe der Erfindung ist es, den beschriebenen Stand der Technik weiterzubilden und aus dem Legierungssystem (Fe1-aMa) 100-x-y-z-α-β-γCuxSiyBzM'αM" βXγ höchstpermeable nanokristalline ) Ringbandkerne für FI-Schalter bereitzustellen, die darüber hinaus großtechnisch effizient und sicher herstellbar sind. Dabei gilt Ma = Co, Ni; 0 ≤ a ≤ 0,5 sowie
- 0,1 ≤ x ≤ 3
- 0 ≤ y ≤ 30
- 0 ≤ z ≤ 25
- 0,1 ≤ α ≤ 30
- 0 ≤ β ≤ 10
- 0 ≤ γ ≤ 10
- M' = Nb, W, Ta, Zr, Hf, Ti, Mo
- M'' = V, Cr, Mn, Al, Pt, Ni, Pd, Y, La, Seltenerdmetalle, Au, Zn, Sn, Re
- X = C, Ge, P, Ga, Sb, In, Be, As
- 0.1 ≤ x ≤ 3
- 0 ≤ y ≤ 30
- 0≤z≤25
- 0.1 ≤ α ≤ 30
- 0 ≤ β ≤ 10
- 0 ≤ γ ≤ 10
- M '= Nb, W, Ta, Zr, Hf, Ti, Mo
- M "= V, Cr, Mn, Al, Pt, Ni, Pd, Y, La, rare earth metals, Au, Zn, Sn, Re
- X = C, Ge, P, Ga, Sb, In, Be, As
Darüber hinaus ist es eine weitere Aufgabe der vorliegenden Erfindung, ein effizientes und großtechnisch realisierbares Verfahren zur Herstellung eines solchen Ringbandkerns anzugeben.Moreover, it is a further object of the present invention to provide an efficient and industrially feasible method for producing such a toroidal core.
Erfindungsgemäß wird diese Aufgabe mit dem Gegenstand der unabhängigen Patentansprüche gelöst. Vorteilhafte Weiterbildungen der Erfindung sind Gegenstand der abhängigen Patentansprüche.According to the invention, this object is achieved with the subject matter of the independent patent claims. Advantageous developments of the invention are the subject of the dependent claims.
Das Ausgangsmaterial dieser Legierungen wird per Schmelzspinntechnologie als zunächst amorphes Band hergestellt. Die daraus gewickelten Ringbandkerne werden einer Wärmebehandlung unterzogen, bei der der amorphe Zustand umschlägt in eine nanokristalline Zweiphasenstruktur mit hervorragenden weichmagnetischen Eigenschaften. Eine wichtige Voraussetzung zur großtechnischen Realisierung höchster Permeabilitätswerte über einen weiten Feldstärkebereich von 1 mA/cm bis über 50 mA/cm ist eine Minimierung der Magnetostriktion (Sättigungsmagnetostriktion) auf Werte |λs | < 6 ppm, besser |λs| < 2,5 ppm, besser |λs| < 1 ppm. Hierzu ist einerseits das Legierungsspektrum einzugrenzen, andererseits ist bei der Wärmebehandlung die Kristallisationstemperatur zur Erzeugung und Reifung des Nanokorns legierungsspezifisch so anzupassen, dass der Volumenanteil der nanokristallinen Phase mit niedrigem, fallweise sogar negativem Magnetostriktionsanteil so stark ausgebildet ist, dass der hohe positive Magnetostriktionsanteil der amorphen Restphase bestmöglich kompensiert wird.The starting material of these alloys is produced by melt spinning technology as a first amorphous band. The wound toroidal cores are subjected to a heat treatment in which the amorphous state turns into a nanocrystalline two-phase structure with excellent soft magnetic properties. An important prerequisite for the industrial realization of highest permeability values over a wide field strength range from 1 mA / cm to over 50 mA / cm is a minimization of the magnetostriction (saturation magnetostriction) to values | λ s | <6 ppm, better | λ s | <2.5 ppm, better | λ s | <1 ppm. For this purpose, on the one hand, the alloy spectrum is limited, on the other hand, in the heat treatment, the crystallization temperature for the generation and maturation of the nanorod is alloy-specifically adapted so that the volume fraction of the nanocrystalline phase with low, occasionally even negative magnetostriction is formed so strong that the high positive magnetostriction of the amorphous residual phase compensated as best as possible.
Gemäß einem Aspekt der Erfindung wird ein Magnetkern für Niederfrequenzanwendungen aus einem spiralförmig aufgewickelten, weichmagnetischen, nanokristallinen Band bereitgestellt, wobei das Band im Wesentlichen die Legierungszusammensetzung
FeRestCOaCubcSidBeCf
aufweist, worin a, b, c, d, e und f in Atomprozent angegeben sind und 0 ≤ a ≤ 1; 0,7 ≤ b ≤ 1,4; 2,5 ≤ c ≤ 3,5; 14,5 ≤ d ≤ 16,5; 5,5 ≤ e ≤ 8 und 0 ≤ f ≤ 1 gilt und Kobalt ganz oder teilweise durch Nickel ersetzt sein kann, wobei der Magnetkern eine Sättigungsmagnetostriktion λs mit |λs < 2 ppm, eine Anfangspermeabilität µ1 µ1 > 100.000 und eine Maximalpermeabilität µmax mit µmax > 600.000 aufweist und auf den Oberflächen des Bandes eine versiegelnde Beschichtung aus Metalloxid angeordnet ist. Das Band weist eine Banddicke d mit d < 24 µm, vorzugsweise d < 21 µm und eine effektive Rautiefe Ra(eff) mit Ra(eff) < 7%, vorzugsweise Ra(eff) < 5% auf.According to one aspect of the invention, a magnetic core for low frequency applications is provided from a spirally wound, soft magnetic, nanocrystalline ribbon, wherein the ribbon is substantially the alloy composition
Fe remainder CO a cub c s d B e C f
wherein a, b, c, d, e and f are in atomic percent and 0 ≤ a ≤ 1; 0.7 ≤ b ≤ 1.4; 2.5 ≤ c ≤ 3.5; 14.5 ≤ d ≤ 16.5; 5.5 ≤ e ≤ 8 and 0 ≤ f ≤ 1 and cobalt may be wholly or partially replaced by nickel, wherein the magnetic core has a saturation magnetostriction λ s with | λ s <2 ppm, an initial permeability μ 1 μ 1 > 100,000 and a Maximum permeability μ max with μ max > 600,000 and is arranged on the surfaces of the tape, a sealing coating of metal oxide. The band has a band thickness d with d <24 μm, preferably d <21 μm and an effective roughness depth R a (eff) with R a (eff) <7%, preferably R a (eff) <5%.
Unter einem Band, das im wesentlichen eine bestimmte Legierungszusammensetzung aufweist, wird hier und im Folgenden ein Band verstanden, dessen Legierung zusätzlich in geringen Konzentrationen fertigungstypische Verunreinigungen anderer Elemente enthalten kann.A strip which essentially has a certain alloy composition is understood here and below to mean a strip whose alloy is additionally embedded in the strip low concentrations may contain impurities typical of other elements.
Unter einer auf den Bandoberflächen angeordneten versiegelnden Beschichtung wird hier und im Folgenden eine Beschichtung verstanden, die ganz überwiegende Teile oder sogar die gesamte Bandoberfläche dicht versiegelt.A sealing coating arranged on the strip surfaces is understood here and below as meaning a coating which tightly seals the predominant parts or even the entire strip surface.
Die Magnetostriktion derartiger Legierungen lässt sich mit einer geeigneten Wärmebehandlung weitestgehend auf Null abgleichen. Dadurch werden die Magnetwerte unempfindlich gegen mechanische Einflüsse, was ein breites Spektrum an Kernformen und Fixierungen erlaubt. Je nach eingesetzter Wärmebehandlung kann die Temperaturcharakteristik der Permeabilität negativ werden, was bei verschiedenen Ausführungsformen von FI-Schaltern von Vorteil sein kann.The magnetostriction of such alloys can be adjusted to zero as far as possible with a suitable heat treatment. As a result, the magnet values are insensitive to mechanical influences, which allows a wide range of core shapes and fixations. Depending on the heat treatment used, the temperature characteristic of the permeability may become negative, which may be advantageous in various embodiments of FI switches.
Zum Nullabgleich der Magnetostriktion wird die Wärmebehandlung vorteilhafterweise so geführt, dass sich die lokalen Magnetostriktionsbeiträge des Nanokorns und der amorphen Restphase bestmöglich ausgleichen.For zero adjustment of the magnetostriction, the heat treatment is advantageously carried out in such a way that the local magnetostriction contributions of the nanorod and of the amorphous residual phase balance as best as possible.
Allerdings hat sich bei Untersuchungen herausgestellt, dass die Bandoberflächen bei den dazu notwendigen Temperaturen von über 540°C eine deutliche Tendenz zu kristallinen Ausscheidungen besitzen. In Abhängigkeit vom Si-, Nb-, B- oder C-Gehalt können diese aus den bekannten FeB2-Phasen bestehen oder aus makrokristallinen Ausscheidungen wie Fe2O3, Fe3O4 und Nb2O5. Deren Entstehung wird begünstigt durch die Rauhigkeit der Bandoberflächen, eine erhöhte Banddicke, einen zu niedrigen Metalloidgehalt, aber auch durch Metall-Gas-Reaktionen zwischen Verunreinigungen im Schutzgas und der Bandoberfläche. Daneben spielt die Entstehung oxidischer Oberflächenschichten beispielsweise aus SiO2 eine wichtige Rolle. Die bei derartigen Oberflächeneffekten entstehenden Kristallanisotropien und Verspannungen führen zu erhöhten feldstärken, niedrigen Remanenzwerten sowie reduzierten Permeabilitätswerten. Die Bildung kristalliner Ausscheidungen kann durch die versiegelnde Beschichtung jedoch vermieden werden.However, investigations have shown that the strip surfaces at the required temperatures of more than 540 ° C have a clear tendency to crystalline precipitates. Depending on the Si, Nb, B or C content, these may consist of the known FeB 2 phases or of macrocrystalline precipitates such as Fe 2 O 3 , Fe 3 O 4 and Nb 2 O 5 . Their formation is favored by the roughness of the strip surfaces, an increased strip thickness, too low a metalloid content, but also by metal-gas reactions between impurities in the protective gas and the strip surface. In addition, the formation of oxidic surface layers, for example of SiO 2, plays an important role. The resulting with such surface effects anisotropies and crystal lead to increased field strengths, low remanence values and reduced permeability values. However, the formation of crystalline precipitates can be avoided by the sealing coating.
Es ist ferner vorteilhaft, bei der großtechnischen Herstellung magnetostriktionsfreier höchstpermeabler Magnetkerne bestimmte Vorgaben zur Legierungszusammensetzung, der Bandgeometrie, der Temperaturführung der Wärmebehandlung sowie der Qualität der Schutzgasatmosphäre einzuhalten.It is also advantageous in the large-scale production of magnetostriction-free highly permeable magnetic cores to observe certain specifications for the alloy composition, the strip geometry, the temperature control of the heat treatment and the quality of the protective gas atmosphere.
Wie sich herausgestellt hat, ist es vorteilhaft, wenn das Band eine Banddicke d mit d < 24 µm, vorzugsweise d < 21 µm aufweist.As has been found, it is advantageous if the strip has a strip thickness d with d <24 μm, preferably d <21 μm.
Das Band weist eine effektive Rautiefe Ra(eff) mit Ra(eff) < 7%, vorzugsweise Ra(eff) < 5% auf. Die effektive Rautiefe wird in der Praxis beispielsweise mittels des Rugotests oder der Tastschnittmethode bestimmt.The band has an effective surface roughness R a (eff) with R a (eff) <7%, preferably R a (eff) <5%. The effective roughness depth is determined in practice, for example by means of the Rugotest or the Tastschnittmethode.
In einer Ausführungsform weist das Band einen Gesamtmetalloidgehalt c+d+e+f > 22,5 at%, vorzugsweise c+d+e+f > 23,5 at% auf.In one embodiment, the tape has a total metal content c + d + e + f> 22.5 at%, preferably c + d + e + f> 23.5 at%.
Gemäß einer Ausführungsform enthält die oxidische Beschichtung Magnesiumoxid. Gemäß einer weiteren Ausführungsform enthält die oxidische Beschichtung Zirkonoxid. Alternativ oder zusätzlich kann die oxidische Beschichtung Oxide eines Elements ausgewählt aus der Gruppe Be, A1, Ti, V, Nb, Ta, Ce, Nd, Gd, weitere Elemente der 2. und 3. Hauptgruppe sowie der Gruppe der Seltenerdmetalle enthalten.In one embodiment, the oxide coating contains magnesia. According to a further embodiment, the oxide coating contains zirconium oxide. Alternatively or additionally, the oxide coating may contain oxides of an element selected from the group consisting of Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, further elements of
Eine derartige Beschichtung des Bandes vor der Wärmebehandlung ermöglicht es, die Wärmebehandlung bei der verhältnismäßig hohen Temperatur durchzuführen, die für die Einstellung der Magnetostriktion notwendig ist, ohne dafür kristalline Ausscheidungen und/oder glasartige Schichten aus SiO2 und damit verbunden eine Verschlechterung der Magnetwerte in Kauf nehmen zu müssen.Such coating of the strip before the heat treatment makes it possible to carry out the heat treatment at the relatively high temperature necessary for the adjustment of the magnetostriction without sacrificing crystalline precipitates and / or vitreous layers of SiO 2 and, associated therewith, deterioration of the magnet values to have to take.
Dieses Vorgehen erlaubt die Herstellung von Magnetkernen mit einer Maximalpermeabilität µmax mit µmax > 500 000, vorzugsweise µmax > 600 000, und einer Anfangspermeabilität µ1 von µ1 > 150 000, vorzugsweise µ1 > 200 000, wobei der Magnetkern ein Remanenzverhältnis BR/BS mit BR/BS > 70% aufweisen kann.This procedure allows the production of magnetic cores having a maximum permeability μ max with μ max > 500,000, preferably μ max > 600,000, and an initial permeability μ 1 of μ 1 > 150,000, preferably μ 1 > 200,000, the magnetic core having a remanence ratio B R / B S with B R / B S > 70%.
Die Sättigungsmagnetostriktion λs kann auf |λs| < 1 ppm, vorzugsweise |λs | < 0,5 ppm abgeglichen sein.The saturation magnetostriction λ s can be reduced to | λ s | <1 ppm, preferably | λ s | <0.5 ppm.
Wegen seiner geringen Magnetostriktion ist der fertige Magnetkern nicht mehr sehr empfindlich gegen Verspannungen. Er kann dann beispielsweise mit einem Haftkleber und/oder mit einem auf einer oder auf beiden Stirnseiten des Magnetkerns polsternd aufgelegten Ring aus einem elastischen Material in einem Schutztrog fixiert sein. Als Kleber können insbesondere Silikonkautschuk, Acrylat oder Silikonfett verwendet werden.Because of its low magnetostriction, the finished magnetic core is no longer very sensitive to tension. It can then be fixed in a protective trough, for example, with a pressure-sensitive adhesive and / or with a ring of an elastic material placed on top of one or both ends of the magnetic core. In particular silicone rubber, acrylate or silicone grease can be used as adhesives.
Zur Fixierung der Bandlagen kann der Magnetkern auf einer oder beiden Stirnseiten eine Epoxi-Wirbelsinterschicht aufweisen.In order to fix the band layers, the magnetic core may have an epoxy vertebral interlayer on one or both end faces.
Gemäß einem Aspekt der Erfindung wird ein solcher Magnetkern in einem Fehlerstromschutzschalter eingesetzt.According to one aspect of the invention, such a magnetic core is used in a residual current circuit breaker.
Gemäß einem Aspekt der Erfindung wird ein Verfahren zur Herstellung eines Magnetkerns für Niederfrequenzanwendungen aus einem spiralförmig aufgewickelten, weichmagnetischen, nanokristallinen Band bereitgestellt, wobei das Band im Wesentlichen die Legierungszusammensetzung
FeRestCOaCubNbcSidBeCf
aufweist, worin a, b, c, d, e und f in Atomprozent angegeben sind und 0 ≤ a ≤ 1; 0,7 ≤ b ≤ 1,4; 2,5 ≤ c ≤ 3,5; 14,5 d ≤ 16,5; 5,5 ≤ e ≤ 8 und 0 ≤ f ≤ 1 gilt und Kobalt ganz oder teilweise durch Nickel ersetzt sein kann. Das Band wird mit einer Beschichtung mit einer Metallalkoxid-Lösung und/oder eines Acetyl-Aceton-Chelatkomplexes mit einem Metall versehen, aus der sich bei einer nachfolgenden Wärmebehandlung zur Nanokristallisation des Bandes eine versiegelnde Beschichtung aus einem Metalloxid bildet. Bei der Wärmebehandlung zur Nanokristallisation des Bandes wird eine Sättigungsmagnetostriktion λs mit | As | < 2 ppm, vorzugsweise | λs | < 1 ppm, vorzugsweise | λs | < 0,5 ppm eingestellt. Die Wärmebehandlung wird in einer Schutzgasatmosphäre aus H2, N2 und/oder Ar durchgeführt, wobei der Taupunkt TP < -25°C oder der Taupunkt TP < -49, 5°C ist.According to one aspect of the invention, there is provided a method of manufacturing a magnetic core for low frequency applications from a spirally wound, soft magnetic, nanocrystalline tape, wherein the tape is substantially the alloy composition
Fe remainder CO a Cu b Nb c Si d B e C f
wherein a, b, c, d, e and f are in atomic percent and 0 ≤ a ≤ 1; 0.7 ≤ b ≤ 1.4; 2.5 ≤ c ≤ 3.5; 14.5 d ≤ 16.5; 5.5 ≤ e ≤ 8 and 0 ≤ f ≤ 1 and cobalt may be wholly or partially replaced by nickel. The tape is provided with a coating of a metal alkoxide solution and / or an acetyl-acetone chelate complex with a metal from which forms a sealing coating of a metal oxide in a subsequent heat treatment for nanocrystallization of the tape. In the heat treatment for nanocrystallization of the ribbon, a saturation magnetostriction λ s with | A s | <2 ppm, preferably | λ s | <1 ppm, preferably | λ s | <0.5 ppm. The heat treatment is carried out in an inert gas atmosphere of H 2 , N 2 and / or Ar, wherein the dew point T P <-25 ° C or the dew point T P <-49, 5 ° C.
Dabei kann als Metall für die Beschichtung vorteilhafterweise ein Element ausgewählt aus der Gruppe Mg, Zr, Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, weitere Elemente der 2. und 3. Hauptgruppe sowie der Gruppe der Seltenerdmetalle verwendet werden.In this case, as the metal for the coating advantageously an element selected from the group Mg, Zr, Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, other elements of the 2nd and 3rd main group and the group of rare earth metals be used.
Zur großtechnischen Herstellung kann dabei folgendermaßen vorgegangen werden, um eine möglichst hohe Permeabilität bei geringer Magnetostriktion zu erzielen:
- Zur Erzielung möglichst vollkommener Feldfreiheit wird die Wärmebehandlung im Durchlaufverfahren feldfrei an ungestapelten Magnetkernen durchgeführt.
- To achieve the best possible field freedom, the heat treatment is carried out in a continuous process field-free on unstacked magnetic cores.
In einer Ausführungsform werden die ungestapelten Magnetkerne während des Durchlaufglühverfahrens auf einem gut wärmeleitenden Träger angeordnet. Ein derartiger Träger besteht beispielsweise aus einem gut wärmeleitenden Metall wie Kupfer, Silber oder gut wärmeleitendem Stahl. Als Träger eignet sich auch ein Bett aus gut wärmeleitendem Keramikpulver.In one embodiment, the unstacked magnetic cores are placed on a good thermal conductivity carrier during the continuous annealing process. Such a carrier consists for example of a good heat-conducting metal such as copper, silver or good heat-conducting steel. The carrier is also a bed of good thermal conductivity ceramic powder.
Beispielsweise können die Ringbandkerne stirnseitig auf Kupferplatten mit einer Stärke von mindestens 4mm, vorzugsweise mindestens 6mm, noch besser mindestens 10mm gesetzt werden. Dies trägt dazu bei, lokale Überhitzungen zu vermeiden, wenn die exotherme Kristallisation einsetzt, in dem die frei werdende Kristallisationswärme effektiv abgeleitet wird.For example, the toroidal cores can be set on the face side to copper plates with a thickness of at least 4mm, preferably at least 6mm, more preferably at least 10mm. This helps to avoid local overheating when the exothermic crystallization sets in, in which the released heat of crystallization is effectively dissipated.
Zusätzlich kann es vorteilhaft sein, wenn der Magnetkern bei der Wärmebehandlung folgende Temperaturzonen durchläuft:
- eine erste Heizzone, in der der Magnetkern auf eine Kristallisationstemperatur aufgeheizt wird;
- eine konstante oder schwach ansteigende Abklingzone mit einer Temperatur geringfügig oberhalb der Kristallisationstemperatur, wobei
die Abklingzone mindestens 10 Minuten lang durchlaufen wird; - eine zweite Heizzone, in der der Magnetkern auf eine Reifungstemperatur zur Einstellung des nanokristallinen Gefüges aufgeheizt wird;
- eine Reifungszone mit einer im Wesentlichen konstanten Reifungstemperatur Tx zwischen 540°C und 600°C, wobei
die Reifungszone mindestens 15 Minuten lang durchlaufen wird.
- a first heating zone in which the magnetic core is heated to a crystallization temperature;
- a constant or slightly rising decay zone having a temperature slightly above the crystallization temperature, wherein the decay zone is passed through for at least 10 minutes;
- a second heating zone in which the magnetic core is heated to a ripening temperature for adjusting the nanocrystalline structure;
- a maturation zone having a substantially constant maturing temperature T x between 540 ° C and 600 ° C, wherein the ripening zone is passed through for at least 15 minutes.
Das Verharren in der Abklingzone dient dazu, die Kristallisationswärme vor einem weiteren Aufheizen des Magnetkerns abklingen zu lassen, um lokale Überhitzungen zu vermeiden.The persistence in the decay zone serves to decay the heat of crystallization before further heating of the magnetic core to avoid local overheating.
Die Wärmebehandlung wird in einer Schutzgasatmosphäre aus H2, N2 und/oder Ar durchgeführt, wobei der Taupunkt TP < -25°C, vorzugsweise TP < -49,5°C ist.The heat treatment is carried out in an inert gas atmosphere of H 2 , N 2 and / or Ar, wherein the dew point T P <-25 ° C, preferably T P <-49.5 ° C.
Um mechanische Spannungen bei nicht vollständig abgeglichener Magnetostriktion möglichst zu vermeiden, wird das Band mit abfallendem Bandzug zu dem Magnetkern gewickelt.In order to avoid mechanical stresses as far as possible when the magnetostriction is not fully balanced, the strip is wound with decreasing strip tension to the magnetic core.
Ausführungsbeispiele der Erfindung werden im folgenden anhand der beigefügten Figuren näher erläutert.
Figur 1- zeigt schematisch einen wechselstromsensitiven FI-Schalter gemäß einer Ausführungsform der Erfindung;
Figur 2- zeigt schematisch einen möglichen Temperaturverlauf einer Wärmebehandlung gemäß einem Verfahren zu Herstellung eines Magnetkerns gemäß einer Ausführungsform der Erfindung;
Figur 3- zeigt die Oberfläche eines unbeschichteten Bandes nach einer Wärmebehandlung;
Figur 4- zeigt ein Diagramm zur Veranschaulichung des Einflusses der Kristallisationstemperatur auf die Änderung der Koerzitivfeldstärke eines Magnetkerns bei radialer Deformation;
Figur 5- zeigt ein Diagramm zur Veranschaulichung des Einflusses der Kristallisationstemperatur und einer Beschichtung auf die µ(H)-Kommutierungskurven eines Magnetkerns;
- Figur 6
- zeigt ein Diagramm zur Veranschaulichung des Einflusses der Kristallisationstemperatur und einer Beschichtung auf die Hystereseschleife eines Magnetkerns;
Figur 7- zeigt eine Sicht auf die Bandunterseite eines unbeschichteten Bandes nach einer Wärmebehandlung;
- Figur 8
- zeigt eine Sicht auf die Bandunterseite eines beschichteten Bandes nach einer Wärmebehandlung;
- Figur 9
- zeigt ein XPS-Tiefenprofil eines unbeschichteten Bandes nach einer Wärmebehandlung;
Figur 10- zeigt eine rasterelektronenmikroskopische Aufnahme einer beschichteten Bandunterseite;
Figur 11- zeigt ein Diagramm zur Veranschaulichung des Einflusses einer Beschichtung auf die Bildung von SiO2-Schichten auf der Bandoberfläche;
- Figur 12
- zeigt ein Diagramm zur Veranschaulichung des Einflusses des Taupunktes der Schutzgasatmosphäre während der Wärmebehandlung auf die Permeabilität;
Figur 13- zeigt ein weiteres Diagramm zur Veranschaulichung des Einflusses des Taupunktes der Schutzgasatmosphäre während der Wärmebehandlung auf die Permeabilität und
- Figur 14
- zeigt ein Diagramm zur Veranschaulichung des Einflusses der effektiven Rautiefe auf die Anfangspermeabilität.
- FIG. 1
- schematically shows an AC-sensitive FI-switch according to an embodiment of the invention;
- FIG. 2
- schematically shows a possible temperature profile of a heat treatment according to a method for manufacturing a magnetic core according to an embodiment of the invention;
- FIG. 3
- shows the surface of an uncoated strip after a heat treatment;
- FIG. 4
- Fig. 12 is a graph showing the influence of the crystallization temperature on the change in the coercive force of a magnetic core when radially deformed;
- FIG. 5
- Fig. 4 is a graph showing the influence of the crystallization temperature and a coating on the μ (H) -commutation curves of a magnetic core;
- FIG. 6
- Fig. 12 is a diagram illustrating the influence of the crystallization temperature and a coating on the hysteresis loop of a magnetic core;
- FIG. 7
- shows a view of the underside of an uncoated strip after heat treatment;
- FIG. 8
- shows a view of the lower surface of a coated strip after a heat treatment;
- FIG. 9
- shows an XPS depth profile of an uncoated belt after a heat treatment;
- FIG. 10
- shows a scanning electron micrograph of a coated belt underside;
- FIG. 11
- shows a diagram illustrating the influence of a coating on the formation of SiO 2 layers on the strip surface;
- FIG. 12
- Fig. 10 is a graph showing the influence of the dew point of the inert gas atmosphere during the heat treatment on the permeability;
- FIG. 13
- shows another diagram for illustrating the influence of the dew point of the inert gas atmosphere during the heat treatment on the permeability and
- FIG. 14
- shows a diagram illustrating the influence of the effective surface roughness on the initial permeability.
Der Vergleich der durch den FI-Schalter 1 fließenden Ströme erfolgt in einem Summenstromwandler 2, durch den die zum und vom Verbraucher fließenden Ströme vorzeichenrichtig addiert werden. Wird im Stromkreis ein Strom gegen Erde abgeleitet, so ist im Summenstromwandler die Summe von hin- und zurückfließendem Strom ungleich Null: es entsteht eine Stromdifferenz, die zum Ansprechen des Fehlerstromschutzschalters 1 und damit zur Abschaltung der Stromzufuhr führt.The comparison of the currents flowing through the FI-
Der Summenstromwandler 2 weist einen Magnetkern 2 auf, der aus einem nanokristallinen weichmagnetischen Band gewickelt ist. Der FI-Schalter 1 umfasst weiter ein Auslöserelais 4, ein vorgespanntes Schaltschloss 5 sowie einen Prüftaster 6 zur manuellen Überprüfung des FI-Schalters 1.The summation
Bei dieser im Durchlaufverfahren durchgeführten Wärmebehandlung wird nach einer anfänglichen Aufheizung des Magnetkerns ein stark verzögerter Anstieg oder sogar ein Temperaturplateau eingesetzt (beide Alternativen sind in
Mit Hilfe einer Vorprobe wird die Temperatur in der Reifungszone so an die Zusammensetzung der jeweiligen Charge angepasst, dass der Betrag des Magnetostriktionswertes minimal wird. Von den einzusetzenden Bandchargen werden dazu zunächst Vorproben hergestellt, die in der Reifungszone unterschiedlichen Temperaturen Tx zwischen 540°C und 600°C ausgesetzt werden. Die anschließende Bestimmung der Magnetostriktion erfolgt entweder direkt an einem entnommenen Bandstück oder indirekt an einem unbeschädigten Kern. Die direkte Messung kann beispielsweise mittels der SAMR-Methode erfolgen. Eine indirekte Methode ist ein Drucktest, bei dem der Umfang des Ringbandkerns beispielsweise um 2% zum Oval verformt wird. Die dabei auftretende Änderung der Koerzitivfeldstärke wird durch Messung der quasistatischen Hystereseschleife mittels eines Remagraphen vor und während der Deformation bestimmt.With the aid of a pre-sample, the temperature in the ripening zone is adapted to the composition of the respective batch so that the magnitude of the magnetostriction value becomes minimal. For this purpose, preliminary samples are first prepared of the strip batches to be used which are exposed to different temperatures T x between 540 ° C. and 600 ° C. in the ripening zone. The subsequent determination of the magnetostriction is carried out either directly on a removed piece of tape or indirectly on an undamaged core. The direct measurement can be done for example by means of the SAMR method. An indirect method is a pressure test in which the circumference of the toroidal core is deformed for example by 2% to the oval. The occurring change in the coercive field strength is determined by measuring the quasi-static hysteresis loop by means of a remainder graph before and during the deformation.
Wie sich aus
Im großtechnischen Produktionsmaßstab lassen sich auf der Basis dieses Verfahrens an einer Legierung wie Fe73,13Co0,17Cu1Nb3Si15,8B6,9 Magnetwerte (bei 50Hz) erzielen, die bei µ1= 120.000-300.000 und µ10 > 450.000 sowie Br/Bs > 70% (quasistatisch gemessen) liegen. Entsprechend
Bei der gleichzeitigen Glühung vieler Kerne im großtechnischen Produktionsmaßstab wird eine große Menge an Feuchtigkeit, die an den Oberflächen der zum Kern gewickelten Bänder anhaftet, in die Ofenanlage eingeschleppt. Dies führt einerseits auf den Bändern zu direkten lokalen korrosiven Oberflächenreaktionen, andererseits diffundiert ein Teil der Feuchtigkeit in die Schutzgasatmosphäre und erhöht dort den Taupunkt in ungünstiger Weise. Unter diesen Bedingungen bilden sich auf den Bandoberflächen kristalline Ausscheidungen, die wie in
Ein weiterer ungünstiger, durch erhöhte Taupunkte begünstigter Oberflächeneffekt, der den kristallinen Ausscheidungen überlagert ist, ist das Aufwachsen einer glasartigen Schicht aus SiO2. Diese ist starr und besitzt einen wesentlich geringeren thermischen Ausdehnungskoeffizienten von 0,45 bis 1 ppm/K als das Bandmetall (ca. 10 ppm/K). Da das Bulkmaterial während der Entstehung und Reifung der nanokristallinen Körner um 1-2% schrumpft, bauen sich mechanische Spannungen auf. Diese führen ebenfalls zu starken Störanisotropien, die die Magnetwerte in unerwünschter Weise beeinflussen.Another unfavorable surface effect favored by increased dew points, which is superimposed on the crystalline precipitates, is the growth of a vitreous layer of SiO 2 . This is rigid and has a much lower thermal expansion coefficient of 0.45 to 1 ppm / K than the band metal (about 10 ppm / K). As the bulk material shrinks by 1-2% during the formation and ripening of the nanocrystalline grains, mechanical stresses build up. These also lead to strong disturbance anisotropies, which influence the magnet values in an undesired manner.
Die in
Der Nachweis für die in den Ofen eingeschleppte Feuchtigkeit erfolgte durch Messung des Taupunktes des H2-Schutzgases mittels des Geräts PANAMETRICS MIS1. Dieser lag vor der Einfahrt der Ringbandkerne in die Heizzone bei -42 °C und stieg während des Durchlaufs auf einen vergleichsweise hohen Wert von -16 °C an. Bedingt durch die Störanisotropien beider überlagerter Oberflächeneffekte waren die Magnetwerte der geglühten Kerne nicht optimal: Die bei 50 Hz gemessenen Losmittelwerte lagen bei <µ1> = 47.873, <µ10> = 222.356, <BR/BS>= 52% sowie <HC> = 28 mA/cm.The moisture introduced into the furnace was detected by measuring the dew point of the H2 protective gas by means of the PANAMETRICS MIS1 device. This was before the entrance of the toroidal cores in the heating zone at -42 ° C and increased during the passage to a relatively high value of -16 ° C. Due to the disturbance anisotropies of both superimposed surface effects, the magnet values of the annealed cores were not optimal: The release mean values measured at 50 Hz were <μ 1 > = 47.873, <μ 10 > = 222.356, <B R / B S > = 52% and < H C > = 28 mA / cm.
Zur Vermeidung derartiger Störeinflüsse hat sich das versiegelnde Beschichten der Bandoberflächen mit einer glühbeständigen Substanz als günstig erwiesen. Geeignet sind gelöste Substanzen, deren Ausgangsstoffe während des Glühprozesses in H2-, N2- oder Ar-Schutzgasatmosphäre oder Gemischen davon bei Temperaturen bis 650 °C zu einer oxidischen, thermisch stabilen Schicht versintern und dabei durch die Wirkung der Schutzgase nicht reduziert werden.In order to avoid such disturbing influences, the sealing coating of the strip surfaces with a heat-resistant substance has proved favorable. Suitable substances are dissolved substances whose starting materials sinter during the annealing process in an H 2 , N 2 or Ar protective gas atmosphere or mixtures thereof at temperatures up to 650 ° C. to form an oxidic, thermally stable layer and are not reduced by the action of the protective gases.
Beispielse für Basismaterialien solcher Beschichtungen sind Be, Mg, Al, Zr, Ti, V, Nb, Ta, Ce, Nd, Gd und andere Elemente der 2. und 3. Hauptgruppe sowie der Gruppe der SE-Elemente. Diese werden als Metallalkoxid-Lösungen im jeweils korrespondierenden Alkohol oder Äther als z.B. Methylat-, Ethylat-, Propylat- oder Butylat-Lösungen im entsprechenden Alkohol oder in Äther gelöste Alkylate oder beispielsweise auch als tri- oder tetra-Isopropylalkoholate auf die Bandoberflächen aufgetragen. Weitere Alternativen sind Acetyl-Aceton-ChelatKomplexe mit den genannten Metallen. Unter dem Einfluss von Luftfeuchtigkeit erfolgt bei der anschließenden Trocknung zwischen 80 °C und 200 °C eine Umwandlung in das jeweilige hydratisierte Hydroxid. Während der späteren Wärmebehandlung wandelt sich dieses unter weiterer Wasserabgabe um in das jeweilige Metalloxid, wodurch eine dichte, fest auf der Oberfläche anhaftende und diese versiegelnde Schutzschicht entsteht. Typische Schichtdicken liegen im Bereich von 0,05 bis 5 µm, wobei eine Schichtdicke im Bereich von 0,2 bis 1 µm hinreichend gute Eigenschaften aufweist und daher in einer Ausführungsform bevorzugt wird.Examples of base materials of such coatings are Be, Mg, Al, Zr, Ti, V, Nb, Ta, Ce, Nd, Gd and other elements of the 2nd and 3rd main groups and the group of SE elements. These are used as metal alkoxide solutions in the respective corresponding alcohol or ether, for example methylate, ethylate, propylate or butylate solutions in the corresponding alcohol or dissolved in ether alkylates or, for example, as tri- or tetra-Isopropylalkoholate applied to the tape surfaces. Other alternatives include acetyl-acetone chelate complexes with the metals mentioned. Under the influence of atmospheric moisture, the subsequent drying between 80 ° C and 200 ° C, a conversion into the respective hydrated hydroxide takes place. During the subsequent heat treatment, this transforms with further release of water in the respective metal oxide, whereby a dense, firmly adhering to the surface and this sealing protective layer is formed. Typical layer thicknesses are in the range of 0.05 to 5 .mu.m, with a layer thickness in the range of 0.2 to 1 .mu.m having sufficiently good properties and therefore being preferred in one embodiment.
Durch die Beschichtung ist es möglich, die Werkstoffeigenschaften bei den für den Nullabgleich der Magnetostriktion notwendigen hohen Temperaturen gegen Oberflächenreaktionen zu stabilisieren. Die dabei anwendungsrelevanten, durch Oberflächeneffekte beeinflussten Kenngrößen sind insbesondere die bei 50 Hz gemessene µ(H) Kennlinie, die quasistatische Koerzitivfeldstärke und die Remanenzinduktion.The coating makes it possible to stabilize the material properties at the high temperatures necessary for the zero adjustment of the magnetostriction against surface reactions. The application-relevant parameters influenced by surface effects are, in particular, the μ (H) characteristic curve measured at 50 Hz, the quasi-static coercive field strength and the remanence induction.
Für das Aufbringen der Lösung als Ausgangsprodukt für die spätere Bildung der versiegelnden Beschichtung existieren zumindest drei mögliche Verfahren. Die genannten Schichtdicken lassen sich jeweils durch Einstellen der Konzentration und über eine Anpassung der Prozessparameter erreichen. Sollen besonders dicke Schichten erzielt werden, kann das Verfahren auch wiederholt werden.There are at least three possible methods for applying the solution as a starting material for the subsequent formation of the sealing coating. The layer thicknesses mentioned can each be achieved by adjusting the concentration and by adapting the process parameters. If particularly thick layers are to be achieved, the process can also be repeated.
In einem möglichen Verfahren wird das Band im Durchlaufverfahren über Umlenkrollen laufend durch das in einer Wanne befindliche Beschichtungsmedium gezogen. Unmittelbar vor dem Aufwickeln zum Kern durchläuft es eine auf 80-200 °C geregelte Trocknungsstrecke. Dieses Verfahren zeichnet sich durch eine besondere Gleichmäßigkeit der Beschichtung aus. Durch wiederholten Durchlauf lassen sich dickere Schichten erzielen.In one possible method, the belt is in a continuous process via pulleys running through the located in a tub Drawn coating medium. Immediately before winding to the core, it passes through a drying section controlled at 80-200 ° C. This process is characterized by a special uniformity of the coating. Repeated cycles allow thicker layers to be achieved.
In einem weiteren möglichen Verfahren wird das nach der Herstellung aufgespulte Band als Spule in die in einem Rezipienten stehende Lösung getaucht und evakuiert. Aufgrund der bei Unterdruck im Bereich des Grobvakuums von 10-300 mbar ausreichend wirksamen Kapillarkräfte dringt die Lösung zwischen die Bandlagen der Spule ein und benetzt die Oberflächen. Die getrockneten Spulen werden anschließend in einem Trockenschrank bei 80-200 °C nachgetrocknet. Das beschichtete Band wird anschließend zu Magnetkernen gewickelt. Dieses Verfahren ist besonders wirtschaftlich.In another possible method, the wound after production tape is dipped as a coil in the standing in a recipient solution and evacuated. Due to the capillary forces which are sufficiently effective at a vacuum in the region of the rough vacuum of 10-300 mbar, the solution penetrates between the band layers of the coil and wets the surfaces. The dried coils are subsequently dried in a drying oven at 80-200 ° C. The coated tape is then wound into magnetic cores. This process is particularly economical.
In einem weiteren möglichen Verfahren werden die aus unbeschichtetem Band gewickelten Kerne in einem Rezipienten in die Lösung getaucht. Nach dem Evakuieren auf den oben genannten Unterdruck dringt die Lösung zwischen die Bandlagen ein und benetzt diese. Die getauchten Kerne werden anschließend bei 80 bis 200 °C in einem Trockenschrank getrocknet. Dieses Verfahren hat den Vorteil, dass der Wickelprozess des Kerns nicht durch das Beschichtungsmedium auf den Bandoberflächen gestört werden kann.In another possible method, the cores wound from uncoated tape are immersed in a recipient in the solution. After evacuation to the above negative pressure, the solution penetrates between the tape layers and wets them. The submerged cores are then dried at 80 to 200 ° C in a drying oven. This method has the advantage that the winding process of the core can not be disturbed by the coating medium on the strip surfaces.
Im Rahmen von Untersuchungen hat sich herausgestellt, dass Beschichtungen mit Magnesium und Zirkon besonders gut verarbeitbar, kostengünstig und prozesssicher sind.Investigations have shown that coatings containing magnesium and zirconium are particularly easy to process, cost-effective and reliable.
Die Konzentration der gelösten Metalle wurde in den verschiedenen organischen Lösungsmitteln in einem weiten Bereich zwischen 0,1 Gew.% und 5 Gew.% variiert, ohne dass nennenswerte Veränderungen in den Magnetwerten auftraten. Allerdings zeigte sich bei sehr niedrigen Konzentrationen eine Zunahme der Streuungen.The concentration of the dissolved metals was varied in the various organic solvents in a wide range between 0.1% by weight and 5% by weight without significant changes in the magnetic values. However, at very low concentrations, there was an increase in scattering.
Zur Überprüfung des Einflusses einer Oberflächenbeschichtung wurden per Schmelzspinntechnologie hergestellte Bänder der Zusammensetzung Fe73,6Co0,1Cu1Nb2,96Si15,45B6,45C0,05 mit der Breite 10 mm in drei Teilmengen gleicher Qualität (Füllfaktor η= 81,0-81,3 %, Ra(eff) = 2,9%) aufgeteilt. Die erste und zweite Teilmenge blieb unbeschichtet, während die dritte Teilmenge in einem Rezipienten im Tauchverfahren mit einer Lösung aus 3,6% Mg-Methylat beschichtet wurde. Das mittels Drehschieberpumpe erzeugte Grobvakuum lag am Ende der Abpumpzeit bei ca. 110 mbar. Nach einer Haltezeit von 15 Minuten wurden die getränkten Spulen für eine Stunde bei 110 °C getrocknet, wodurch sich eine anhaftende Schicht aus hydratisiertem Mg(OH)2 der Stärke 0,8 µm bildete.To check the influence of a surface coating, strips of the composition Fe 73.6 Co 0.1 Cu 1 Nb 2.96 Si 15.45 B 6.45 C 0.05 with a width of 10 mm, produced by melt-spinning technology, were prepared in three aliquots of the same quality ( Fill factor η = 81.0-81.3%, R a (eff) = 2.9%). The first and second aliquots remained uncoated while the third aliquot in a recipient was immersion coated with a solution of 3.6% Mg methylate. The rough vacuum generated by means of a rotary vane pump was approx. 110 mbar at the end of the pumpdown time. After a holding time of 15 minutes, the impregnated coils were dried for one hour at 110 ° C, forming an adherent layer of hydrated Mg (OH) 2 of 0.8 microns thickness.
Anschließend wurden sowohl die beschichteten als auch die unbeschichteten Bänder mit abfallendem Bandzug zu verspannungsfreien Ringbandkernen der Abmessung 32 mm mal 16 mm mal 10 mm gewickelt. Zur Vorbereitung der Wärmebehandlung wurden jeweils 100 Kerne stirnseitig auf quadratische Kupferplatten der Abmessung 300 mm mal 300 mm mal 6 mm gesetzt.Subsequently, both the coated and the uncoated strips were wound with decreasing strip tension to tension-free ring band cores of the dimension 32 mm by 16 mm by 10 mm. For the preparation of the heat treatment, 100 cores were placed on the face side on square copper plates measuring 300 mm by 300 mm by 6 mm.
Die anschließende Wärmebehandlung erfolgte vollkommen feldfrei im Durchlaufverfahren mit einem Temperaturverlauf ähnlich wie in
Zur Vermeidung von Überhitzungen, die in Verbindung mit atmosphärischen Verunreinigungen zu verstärkten Oberflächenreaktionen und damit zu Störanisotropien führen können, wurde die Reifungszone beim ersten Drittel der Kerne aus unbeschichtetem Band möglichst niedrig auf Tx = 520 °C eingestellt. Die bei 50 Hz gemessenen µ(H)-Kennlinie sowie die quasistatisch (f = 0,01 Hz) gemessenen Hystereseschleifen in den
Zum Schutz gegen mechanische Verspannungen durch Handlings- oder Weiterverarbeitungsschritte wie die Bewicklung mit Draht oder Litze wurden diese Kerne mit Silikonkautschuk als Kleber stirnseitig in Ultramidtröge eingeklebt. Aufgrund der mittels SAMR gemessenen Magnetostriktion von λs ≈ 8 ppm erhöhte sich durch den zwischen die Bandlagen eindringenden Kleber die quasistatische Koerzitivfeldstärke von HC = 3,9 mA/cm auf 8,6 mA/cm, wobei gleichzeitig die bei 50 Hz gemessene Maximalpermeabilität auf µ16 = 373.242 und BR/BS auf 59% zurückgingen. Derartige Kerne waren aufgrund zu niedriger Permeabilitäten in FI-Schaltern nicht gut einsetzbar.To protect against mechanical tension caused by handling or further processing steps such as wire or wire wrapping, these cores were glued with silicone rubber as an adhesive in the front of Ultramidtröge. Due to the means By SAMR measured magnetostriction of λ s ≈ 8 ppm increased by the adhesive penetrating between the tape layers, the quasi-static coercive field strength of H C = 3.9 mA / cm to 8.6 mA / cm, at the same time measured at 50 Hz maximum permeability to μ 16 = 373,242 and B R / B S dropped to 59%. Such cores were not well used due to low permeabilities in FI switches.
Das zweite Drittel der Kerne, die ebenso wie das erste Drittel unbeschichtet waren, wurde mit der in der Vorprobe für optimal für den Nullabgleich der Magnetostriktion befundenen Temperatur von Tx = 575 °C auf λs ≈ 0 ppm geglüht.The second third of the cores, which were uncoated as well as the first third, were annealed with the temperature of T x = 575 ° C, found in the pre-sample to be optimally zero magnetostrictive, to λ s ≈ 0 ppm.
Dabei ging allerdings die Maximalpermeabilität zurück auf µ28 = 221.435, wobei die quasistatisch gemessene Koerzitivfeldstärke mit HC = 13,2 mA/cm sehr hoch lag, siehe
Zur Analyse der Ursache für diese Verschlechterung wurden die Bandoberflächen der Kerne mittels Lichtmikroskopie untersucht. Wie in
Das mit der 3,6%igen Lösung aus Mg-Methylat beschichtete letzte Drittel der Kerne zeigte dagegen nach einer Glühung bei Tx = 575 °C, wie in den
Wie die rasterelektronenmikroskopische Untersuchung der Bandoberfläche in
Im Verlauf der Untersuchungen wurde der Taupunkt des H2- und N2-Schutzgases als weiterer kritischer Parameter bei der Herstellung höchstpermeabler, magnetostriktionsfreier Magnetkerne aufgedeckt. Dieser wird um so bedeutungsvoller, je höher die zum Abgleich der Magnetostriktion notwendige Temperatur wird. Zur Untersuchung dieses Effektes wurden im feldfreien Durchlaufofen eine große Zahl an Testglühungen an jeweils einem Ensemble von 100 Kernen der Abmessung 26 mm mal 10 mm mal 6 mm aus Band der Zusammensetzung Fe73,13CO0,17Cu1Nb3Si15,8B6,9 durchgeführt. Die hierbei eingesetzten Bänder besaßen eine effektive Rautiefe Ra(eff) von etwa 3% und einen Füllfaktor um 81,5 %. Der Fertigungsgang der Kerne erfolgte nach demselben Muster wie bereits beschrieben. Das gesamte Band wurde mit einer Lösung aus 2,4%igem Mg-Methylat beschichtet.In the course of the investigations, the dew point of the H 2 and N 2 protective gas became another critical parameter in the production of highly permeable magnetostriction-free magnetic cores uncovered. This becomes all the more meaningful the higher the temperature needed to balance the magnetostriction becomes. To investigate this effect, a large number of test anneals were carried out in a field-free continuous furnace on an ensemble of 100 cores measuring 26 mm by 10 mm by 6 mm from the composition Fe 73.13 CO 0.17 Cu 1 Nb 3 Si 15.8 B 6.9 . The tapes used had an effective surface roughness R a (eff) of about 3% and a fill factor of 81.5%. The production of the cores was carried out according to the same pattern as already described. The entire tape was coated with a solution of 2.4% Mg-methylate.
Bei den Wärmebehandlungen wurde durch Mischen von angefeuchtetem und trockenem H2-Gas der Taupunkt zwischen -20 °C und -55 °C variiert. Zur Messung des Taupunktes wurde das Gerät PANAMETRICS MIS1 eingesetzt.In the heat treatments, the dew point was varied between -20 ° C and -55 ° C by mixing humidified and dry H 2 gas. To measure the dew point the device PANAMETRICS MIS1 was used.
In diesem Atmosphären wurden die Testkerne mit demselben Temperaturprofil auf Kupferplatten geglüht, wie es bereits oben in Ergänzung zu
In einem zweiten Durchgang wurde die zuvor in einer Vorprobe ermittelte, für den Magnetostriktionsabgleich optimale Temperatur Tx = 570 °C eingestellt. Die Mittelwerte der bei 50 Hz und einer Feldstärke von 11,27 mA/cm gemessenen Permeabilitäten sind in
In einer weiteren Versuchsreihe zur Eingrenzung der Einflussparameter wurde auf der Schmelzspinanlage solange Band der Zusammensetzung Fe73,13Co0,17Cu1Nb3Si15,8B6,9 in der Breite 6 mm gegossen, bis die ursprünglich nahezu perfekte Oberfläche der Gießwalze starke Verschleißspuren aufwies. Durch diesen Spurverschleiß entstand längs des Bandverlaufs ein kontinuierlicher Qualitätsabfall, der sich in einer Zunahme der Oberflächenrauheit manifestierte. Das gegossene Band wurde zu ungefähr gleich großen Spulen aufgewickelt, wobei jeweils von Anfang, Mitte und Ende einer Spule eine Bandprobe entnommen wurde. An diesen wurde taktil mittels Querschriebverfahren auf beiden Oberflächen die Rautiefe Ra gemessen, sowie die mittlere Banddicke aus spezifischem Gewicht (as cast 7,07 g/cm3), Länge, Breite und Gewicht der Bandprobe errechnet. Schließlich wurden die effektiven Rautiefen Ra(eff) der Bandproben durch Division der Summe der Ra-Werte beider Oberflächen durch die Banddicke bestimmt.In a further series of experiments to limit the influencing parameters, a tape of the composition Fe 73.13 Co 0.17 Cu 1 Nb 3 Si 15.8 B 6.9 with a width of 6 mm was cast on the melt spinning plant until the originally almost perfect surface of the Casting wheel had strong signs of wear. This track wear resulted in a continuous drop in quality along the belt, manifested in an increase in surface roughness. The cast strip was wound into approximately equal size bobbins, with a tape sample taken from each of the beginning, middle and end of a bobbin. At this length, width and weight of the tape sample was the tactile surface roughness R a as measured by cross-Wrote method on both surfaces, and the average strip thickness of the specific weight (as cast 7.07 g / cm 3) is calculated. Finally, the effective roughnesses R a (eff) of the tape samples were determined by dividing the sum of the R a values of both surfaces by the tape thickness.
Die vollständig aufgewickelten Spulen wurden dreifach im Durchlaufverfahren mit einer Lösung aus 1,9%igem Zr-Tetraisopropylalkoholat beschichtet und anschließend für eine Stunde bei 130 °C getrocknet. Anschließend wurde das gesamte Band spannungsfrei zu Kernen der Abmessung 26 mm mal 10 mm mal 6 mm gewickelt, wobei die Reihenfolge der Kerne und die Zuordnung zu den ursprünglichen Spulen festgehalten wurde. Dadurch wurde es möglich, bestimmten Kernen Positionen innerhalb der Spulen und damit einen Wert für Ra(eff) zuzuordnen. Nach stirnseitigem Aufsetzen von jeweils 50 Kernen auf quadratische Kupferplatten der Abmessung 300 mm mal 300 mm mal 6 mm erfolgte eine Durchlaufglühung mit dem bereits beschriebenen Temperaturprofil mit einer Reifungstemperatur Tx = 570 °C.The fully wound coils were coated three times in a continuous process with a solution of 1.9% Zr tetraisopropyl alcoholate and then dried for one hour at 130 ° C. Subsequently, the entire band was wound stress-free to cores of dimension 26 mm by 10 mm by 6 mm, wherein the order of the cores and the Assignment to the original coils was recorded. This made it possible to assign positions within the coils to certain cores and thus a value for R a (eff). After frontal placing of each 50 cores on square copper plates measuring 300 mm by 300 mm by 6 mm was carried out a continuous annealing with the already described temperature profile with a maturation temperature T x = 570 ° C.
Zur Bestimmung der von der Bandgeometrie abhängigen Anfangspermeabilität wurden an den Kernen die µ1-Werte bei 50 Hz gemessen und in
In der beschriebenen Versuchsreihe erfolgte die Glühung bei einem Taupunkt von -53 °C und Tx = 570 °C, was nach Ausweis einer SAMR-Magnetostriktionsmessung zu λs = 0,1 ppm führte. Demzufolge konnten die Kerne mittels Silikonkautschuk in einem Kunststofftrog eingeklebt oder mittels eines mechanisch dämpfenden Schaumgummirings lose in einen Schutztrog aus Kunststoff oder Metall eingesetzt werden, ohne dass die Permeabilität in nennenswerter Weise verändert wurde.In the series of experiments described, the annealing was carried out at a dew point of -53 ° C. and T x = 570 ° C., which led to λ s = 0.1 ppm after detection of a SAMR magnetostriction measurement. As a result, the cores could be glued into a plastic trough by means of silicone rubber or loosely inserted into a plastic or metal protective trough by means of a mechanically dampening foam rubber ring, without any appreciable change in permeability.
Die Ergebnisse der Untersuchungen sind in Tabelle 1 zusammengefasst. Dabei bedeutet die Markierung *) eine Fixierung mit Silikonkautschuk und die Markierung **) eine nicht verspannende Fixierung mit einem hochviskosen Acrylatkleber.The results of the investigations are summarized in Table 1. The marking *) means a fixation with silicone rubber and the marking **) a non-tensioning fixation with a high-viscosity acrylate adhesive.
Claims (16)
- A magnetic core for low-frequency applications comprising a spirally wound, soft magnetic nanocrystalline tape, wherein the tape has the alloy composition
FeresidueCoaCubNbcSidBeCf,
in which a, b, c, d, e and f are given as atomic percentages and 0 ≤ a 1; 0.7 b ≤ 1.4; 2.5 ≤ c ≤ 3.5; 14.5 ≤ d ≤ 16.5; 5.5 ≤ e ≤ 8 and 0 ≤ f ≤ 1, and cobalt may be fully or partially substituted with nickel,
wherein the magnetic core has a saturation magnetostriction λs of λs < 2 ppm, an initial permeability µ1 of µ1 > 100 000 and a maximum permeability µmax of µmax > 600 000, wherein the tape has a tape thickness d of d < 24 µm, preferably d < 21 µm, and an effective surface roughness Ra(eff) of Ra(eff) < 7%, preferably Ra(eff) < 5%, and wherein a sealing coating of metal oxide is arranged on the surfaces of the tape. - The magnetic core according to claim 1, wherein the oxidic coating contains magnesium oxide and/or zirconium oxide and/or oxides of an element selected from the group comprising Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, and additional elements from the 2end and 3rd main groups and from the rare earth metals group.
- The magnetic core according to claim 1 or 2, wherein the magnetic core has an initial permeability µ1 of µ1 > 150 000, preferably µ1 > 200 000.
- The magnetic core according to any one of claims 1 to 3, wherein the magnetic core has a saturation magnetostriction λs of λs < 1 ppm, preferably λs < 0.5 ppm.
- The magnetic core according to any one of claims 1 to 4, wherein the tape has a total metalloid content c+d+e+f > 22.5 at%, preferably c+d+e+f > 23.5 at%.
- The magnetic core according to any one of claims 1 to 5, wherein the magnetic core has a remanence ratio BR/BS of BR/BS > 70%.
- The magnetic core according to any one of claims 1 to 6, which is secured in a protective trough with a pressure-sensitive adhesive and/or with a ring made of an elastic material placed as cushioning at one or both end faces of the magnetic core.
- The magnetic core according to any one of claims 1 to 6, which has a fluidized bed epoxy coating on one or both end faces, which fixes the tape layers.
- A residual current circuit breaker having a magnetic core according to any one of claims 1 to 8.
- A method for producing a magnetic core for low-frequency applications according to any one of claims 1 to 8, wherein the tape is provided with a coating having a metal alkoxide solution and/or an acetylacetonate chelate complex with a metal, from which coating a sealing coating of metal oxide forms during a subsequent heat treatment for nanocrystallizing the tape, and wherein during the heat treatment for nanocrystallizing the tape, a saturation magnetostriction λs of |λs| < 2 ppm is established, and wherein the heat treatment is carried out in a protective gas atmosphere of H2, N2 and/or Ar, in which the saturation temperature TP is < -25°C or the saturation temperature TP is < 49.5°C.
- The method according to claim 10, wherein an element selected from the group comprising Mg, Zr, Be, Al, Ti, V, Nb, Ta, Ce, Nd, Gd, and additional elements from the 2nd and 3rd main groups and from the rare earth metals group is used as the metal for the coating.
- The method according to claim 10 or 11, wherein during the heat treatment, a saturation magnetostriction λs of | λs | < 1 ppm, preferably of |λs| < 0.5 ppm is established.
- The method according to any one of claims 10 to 12, wherein the heat treatment is carried out field-free in a continuous annealing process on unstacked magnetic cores.
- The method according to claim 13, wherein the unstacked magnetic cores are arranged on a highly thermally conductive support during the continuous annealing process.
- The method according to claim 13 or 14, wherein the magnetic core passes through the following temperature zones during heat treatment:- a first heating zone in which the magnetic core is heated to a crystallization temperature;- a constant or slightly increasing subsidence zone in which the temperature is slightly above the crystallization temperature, wherein the passage through the subsidence zone lasts at least 10 minutes;- a second heating zone in which the magnetic core is heated to a ripening temperature to establish the nanocrystalline structure;- a ripening zone having a substantially constant ripening temperature Tx of between 540°C and 600°C, wherein the passage through the ripening zone lasts at least 15 minutes.
- The method according to any one of claims 10 to 15, wherein the tape is wound to the magnetic core with decreasing tape tension.
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CN201180038894.8A CN103069512B (en) | 2010-08-06 | 2011-08-05 | Magnetic core and the method preparing the magnetic core for low frequency applications for low frequency applications |
JP2013522339A JP2013532910A (en) | 2010-08-06 | 2011-08-05 | Magnetic core for low frequency applications and method of manufacturing a magnetic core for low frequency applications |
US13/814,457 US20130214893A1 (en) | 2010-08-06 | 2011-08-05 | Magnet core for low-frequency applications and method for producing a magnet core for low-frequency applcations |
US15/214,138 US10892090B2 (en) | 2010-08-06 | 2016-07-19 | Magnet core for low-frequency applications and method for producing a magnet core for low-frequency applications |
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CN105074843B (en) * | 2013-02-15 | 2018-06-08 | 日立金属株式会社 | It has used the ring-shaped magnetic core of Fe base nanometer crystal body non-retentive alloys and has used its magnetic part |
KR20150143251A (en) * | 2014-06-13 | 2015-12-23 | 삼성전기주식회사 | Core and coil component having the same |
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CN108231315A (en) * | 2017-12-28 | 2018-06-29 | 青岛云路先进材料技术有限公司 | A kind of iron cobalt-based nanometer crystal alloy and preparation method thereof |
CN110060831B (en) * | 2019-05-13 | 2021-01-29 | 安徽升隆电气有限公司 | Preparation process of anti-direct current transformer iron core |
CN110767399A (en) * | 2019-10-25 | 2020-02-07 | 中磁电科有限公司 | Composite magnetic material and manufacturing method thereof |
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DE10045705A1 (en) * | 2000-09-15 | 2002-04-04 | Vacuumschmelze Gmbh & Co Kg | Magnetic core for a transducer regulator and use of transducer regulators as well as method for producing magnetic cores for transducer regulators |
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PL1710812T3 (en) | 2005-02-25 | 2008-12-31 | Magnetec Gmbh | Fault-current circuit breaker and magnetic core for a fault-current circuit breaker |
JP5182601B2 (en) * | 2006-01-04 | 2013-04-17 | 日立金属株式会社 | Magnetic core made of amorphous alloy ribbon, nanocrystalline soft magnetic alloy and nanocrystalline soft magnetic alloy |
DE102006019613B4 (en) * | 2006-04-25 | 2014-01-30 | Vacuumschmelze Gmbh & Co. Kg | Magnetic core, process for its preparation and its use in a residual current circuit breaker |
US20070273467A1 (en) * | 2006-05-23 | 2007-11-29 | Jorg Petzold | Magnet Core, Methods For Its Production And Residual Current Device |
DE102007034532A1 (en) * | 2007-07-24 | 2009-02-05 | Vacuumschmelze Gmbh & Co. Kg | Magnetic core, process for its production and residual current circuit breaker |
JP5339192B2 (en) * | 2008-03-31 | 2013-11-13 | 日立金属株式会社 | Amorphous alloy ribbon, nanocrystalline soft magnetic alloy, magnetic core, and method for producing nanocrystalline soft magnetic alloy |
-
2010
- 2010-08-06 EP EP10172135.5A patent/EP2416329B1/en active Active
-
2011
- 2011-08-05 US US13/814,457 patent/US20130214893A1/en not_active Abandoned
- 2011-08-05 CN CN201180038894.8A patent/CN103069512B/en active Active
- 2011-08-05 WO PCT/IB2011/053515 patent/WO2012017421A1/en active Application Filing
- 2011-08-05 JP JP2013522339A patent/JP2013532910A/en active Pending
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2016
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CN103069512B (en) | 2016-11-02 |
US20170011846A1 (en) | 2017-01-12 |
WO2012017421A1 (en) | 2012-02-09 |
EP2416329A1 (en) | 2012-02-08 |
CN103069512A (en) | 2013-04-24 |
US20200227204A9 (en) | 2020-07-16 |
JP2013532910A (en) | 2013-08-19 |
US20130214893A1 (en) | 2013-08-22 |
US10892090B2 (en) | 2021-01-12 |
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