EP2695171B1 - Nouvelle composition de poudre composite à base de fer, et méthode de fabrication d'un composant de poudre - Google Patents

Nouvelle composition de poudre composite à base de fer, et méthode de fabrication d'un composant de poudre Download PDF

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EP2695171B1
EP2695171B1 EP12713715.6A EP12713715A EP2695171B1 EP 2695171 B1 EP2695171 B1 EP 2695171B1 EP 12713715 A EP12713715 A EP 12713715A EP 2695171 B1 EP2695171 B1 EP 2695171B1
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Prior art keywords
iron
based powder
powder
layer
composite iron
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German (de)
English (en)
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EP2695171A2 (fr
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Zhou Ye
Hanna Staffansson
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Hoganas AB
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Hoganas AB
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0207—Using a mixture of prealloyed powders or a master alloy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • 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
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • H01F1/20—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 in the form of particles, e.g. powder
    • H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • 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
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component

Definitions

  • the present invention concerns a soft magnetic composite powder material for the preparation of soft magnetic components as well as the soft magnetic components which are obtained by using this soft magnetic composite powder. Specifically the invention concerns such powders for the preparation of soft magnetic components materials working at high frequencies, the components suitable as inductors or reactors for power electronics.
  • Soft magnetic materials are used for various applications, such as core materials in inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
  • soft magnetic cores such as rotors and stators in electric machines, are made of stacked steel laminates.
  • Soft magnetic composites may be based on soft magnetic particles, usually iron-based, with an electrically insulating coating on each particle. By compacting the insulated particles optionally together with lubricants and/or binders using the traditionally powder metallurgy process, soft magnetic components may be obtained.
  • the present invention relates to an iron-based soft magnetic composite powder, the core particles thereof being coated with a carefully selected coating rendering the material properties suitable for production of inductors through compaction of the powder followed by a heat treating process.
  • An inductor or reactor is a passive electrical component that can store energy in form of a magnetic field created by the electric current passing through said component.
  • An inductors ability to store energy, inductance (L) is measured in henries (H).
  • an inductor is an insulated wire winded as a coil.
  • An electric current flowing through the turns of the coil will create a magnetic field around the coil, the field strength being proportional to the current and the turns/length unit of the coil.
  • a varying current will create a varying magnetic field which will induce a voltage opposing the change of current that created it.
  • Ferromagnetic- or iron- core inductors use a magnetic core made of a ferromagnetic or ferrimagnetic material such as iron or ferrite to increase the inductance of a coil by several thousand by increasing the magnetic field, due to the higher permeability of the core material.
  • the magnetic permeability, ⁇ , of a material is an indication of its ability to carry a magnetic flux or its ability to become magnetised. Permeability is defined as the ratio of the induced magnetic flux, denoted B and measured in newton/ampere*meter or in volt*second/meter 2 , to the magnetising force or field intensity, denoted H and measured in amperes/meter, A/m. Hence magnetic permeability has the dimension volt*second/ampere*meter.
  • Permeability may also be expressed as the inductance per unit length, henries/meter.
  • Magnetic permeability does not only depend on material carrying the magnetic flux but also on the applied electric field and the frequency thereof. In technical systems it is often referred to the maximum relative permeability which is maximum relative permeability measured during one cycle of the varying electrical field.
  • An inductor core may be used in power electronic systems for filtering unwanted signals such as various harmonics.
  • DC- bias may be expressed in terms of percentage of maximum incremental permeability at a specified applied magnetic field, e.g. at 4 000 A/m.
  • Coatings of organic materials are known from e.g. the U.S. Pat. No. 5,595,609 .
  • Coatings comprising both inorganic and organic material are known from e.g. the U.S. Pat. Nos. 6,372,348 and 5,063,011 and the DE patent publication 3,439,397 , according to which publication the particles are surrounded by an iron phosphate layer and a thermoplastic material.
  • European Patent EP1246209B1 describes a ferromagnetic metal based powder wherein the surface of the metal-based powder is coated with a coating consisting of silicone resin and fine particles of clay minerals having layered structure such as bentonite or talc.
  • US6,756,118B2 reveals a soft magnetic powder metal composite comprising a least two oxides encapsulating powdered metal particles, the at least two oxides forming at least one common phase.
  • the patent application JP2002170707A describes an alloyed iron particle coated with a phosphorous containing layer, the alloying elements may be silicon, nickel or aluminium.
  • the coated powder is mixed with a water solution of sodium silicate followed by drying. Dust cores are produced by moulding the powder and heat treat the moulded part in a temperature of 500-1000°C.
  • Sodium silicate is mentioned in JP51-089198 as a binding agent for iron powder particles when producing dust cores by moulding of iron powder followed by heat treating of the moulded part.
  • US 6 903 641 B2 discloses a process for producing a powder magnetic core comprising Sendust (Fe-9Si-6Al) powder and pure iron powder, both coated with a phosphate-based insulation film formed into a die compacted at ⁇ 700 MPa and annealing in the air at 300-500 °C.
  • a compacted component formed of a Fe-13Cr powder coated with a phosphoric acid film and further coated with a waterglass/Kibushi clay (a form of kaolin clay) insulation film, press-formed at 980-2450 MPa and heat-treated after compaction at 650 °C is shown in JP 2003 124016 A .
  • the present invention has been done in view of the need for powder cores which are primarily intended for use at higher frequencies, i.e. frequencies above 2 kHz and particularly between 5 and 100 kHz, where higher resistivity and lower core losses are essential.
  • the saturation flux density shall be high enough for core downsizing.
  • it is an especial advantage of the present invention that it is not necessary to use any organic binding agent in the powder composition, which powder composition is later compacted in the compaction step.
  • Heat treatment of the green compact can therefore be performed at higher temperature without the risk that any organic binding agent decomposes; a higher heat treatment temperature will also improve the flux density and decrease core losses.
  • the absence of organic material in the final, heat treated core also allows the core to be used in environments with elevated temperatures without risking decreased strength due to softening and decomposition of an organic binder, and improved temperature stability is thus achieved.
  • An object of the invention is to provide a new iron- based composite powder comprising a core of an iron based powder the surface thereof coated with a new composite electrical insulated coating.
  • the new iron based composite powder being especially suited to be used for production of inductor cores for power electronics.
  • Another object of the invention is to provide a method for producing such inductor cores.
  • the present invention provides an iron powder mixture and process methods for treating said mixture which can be used to prepare e.g. inductors having high saturation flux density, lower core loss, and the manufacturing process thereof can be simplified.
  • the composition is a composite iron-based powder composition
  • core particles coated with a layer containing an alkaline silicate combined with a clay mineral containing a phyllosilicate, wherein the combined silicon-oxygen tetrahedral layer and hydroxide octahedral layers thereof preferably are electrically neutral, wherein the core particles is a mixture of
  • the sendust particles are coated with a phosphorous containing layer prior to coating with said alkaline silicate combined with a clay mineral containing a phyllosilicate.
  • this coating may be termed "alkaline silicate-coating", or “clay-coating”.
  • This coating may be e.g. kaolin- or talc-based.
  • the atomized particles are coated with a phosphorous containing layer prior to coating with said alkaline silicate coating.
  • the terms "layer” and “coating” may be used interchangeably.
  • the iron particles may be in the form of a pure iron powder having low content of contaminants such as carbon or oxygen.
  • the iron content is preferably above 99.0% by weight, however it may also be possible to utilise iron-powder alloyed with for example silicon.
  • the powders contain besides iron and possible present alloying elements, trace elements resulting from inevitable impurities caused by the method of production. Trace elements are present in such a small amount that they do not (or only marginally) influence the properties of the material. Examples of trace elements may be carbon up to 0.1 %, oxygen up to 0.3%, sulphur and phosphorous up to 0.3 % each and manganese up to 0.3%.
  • the particle size of the iron- based powder is determined by the intended use, i.e. which frequency the component is suited for.
  • the mean particle size of the iron-based powder which is also the mean size of the coated powder as the coating is very thin, may be between 20 to 300 ⁇ m.
  • suitable iron-based powders are e.g. 20-80 ⁇ m, a so called 200 mesh powder, 70-130 ⁇ m, a 100 mesh powder, or 130-250 ⁇ m, a 40 mesh powder.
  • the iron alloy particles may consist essentially of 7% to 13% by weight silicon, 4% to 7% by weight aluminium, the balance being iron, the remainder being impurities.
  • sendust Such a powder is known in the field as sendust.
  • sendust essentially contains 84-86%Fe, 9-10%Si and 5-6%Al, on a weight basis.
  • the iron particles may be water atomized or gas atomized. Methods for atomizing iron are known in the literature.
  • the phosphorous containing coating which is normally applied to the bare iron-based powder may be applied according to the methods described in US patent 6,348,265 .
  • the amount of added solution depends inter alia on the particle size of the powder; however the amount shall be sufficient in order to obtain a coating having a thickness between 20 and 300 nm.
  • a thin phosphorous containing coating by mixing an iron-based powder with a solution of ammonium phosphate dissolved in water or using other combinations of phosphorous containing substances and other solvents.
  • the resulting phosphorous containing coating cause an increase in the phosphorous content of the iron-based powder of between 0.01 to 0.15%.
  • the alkaline silicate coating is applied to the phosphorous coated iron-based powder by mixing the powder with particles of a clay or a mixture of clays containing defined phyllosilicate and a water soluble alkaline silicate, commonly known as water glass, followed by a drying step at a temperature between 20-250°C or in vacuum.
  • Phyllosilicates constitutes the type of silicates where the silicontetrahedrons are connected with each other in the form of layers having the formula (Si 2 O 5 2- ) n . These layers are combined with at least one octahedral hydroxide layer forming a combined structure.
  • the octahedral layers may for example contain either aluminium or magnesium hydroxides or a combination thereof. Silicon in the silicontetrahedral layer may be partly replaced by other atoms. These combined layered structures may be electroneutral or electrically charged, depending on which atoms are present.
  • the type of phyllosilicate is of vital importance in order to fulfil the objects of the present invention.
  • the phyllosilicate shall be of the type having uncharged or electroneutral layers of the combined silicontetrahedral- and hydroxide octahedral - layer.
  • Examples of such phyllosilicates are kaolinite present in the clay kaolin, pyrofyllit present in phyllite, or the magnesium containing mineral talc.
  • the mean particle size of the clays containing defined phyllosilicates shall be below 15, preferably below 10, preferably below 5 ⁇ m, even more preferable below 3 ⁇ m.
  • the amount of clay containing defined phyllosilcates to be mixed with the coated iron-based powder shall be between 0.2-5%, preferably between 0.5-4%, by weight of the coated composite iron- based powder.
  • the amount of alkaline silicate calculated as solid alkaline silicate to be mixed with the coated iron-based powder shall be between 0.1-0.9% by weight of the coated composite iron- based powder, preferably between 0.2-0.8% by weight of the iron-based powder. It has been shown that various types of water soluble alkaline silicates can be used, thus sodium, potassium and lithium silicate can be used. Commonly an alkaline water soluble silicate is characterised by its ratio, i.e.
  • the molar ratio of the water soluble alkaline silicate shall be 1.5-4, both end points included. If the molar ratio is below 1.5 the solution becomes too alkaline, if the molar ratio is above 4 SO 2 will precipitate. It may be possible to omit the second kaolin - sodium silicate coating on the Sendust particles and still achieve excellent magnetic properties. However, in order to further enhance the magnetic properties the second coating layer should cover both the Sendust and the iron powder.
  • the alkaline silicate (or clay) coating may be replaced by a metal-organic coating (second coating)
  • at least one metal-organic layer is located outside the first phosphorous-based layer.
  • the metal-organic layer is of a metal-organic compound having the general formula: R 1 [(R 1 ) x (R 2 ) y (M)] n O n-1 R 1 wherein:
  • the metal-organic compound may be selected from the following groups: surface modifiers, coupling agents, or cross-linking agents.
  • R 1 in the metal-organic compound may be an alkoxy-group having less than 4, preferably less than 3 carbon atoms.
  • R 2 is an organic moiety, which means that the R 2 -group contains an organic part or portion.
  • R 2 may include 1-6, preferably 1-3 carbon atoms.
  • R 2 may further include one or more hetero atoms selected from the group consisting of N, O, S and P.
  • the R 2 group may be linear, branched, cyclic, or aromatic.
  • R 2 may include one or more of the following functional groups: amine, diamine, amide, imide, epoxy, hydroxyl, ethylene oxide, ureido, urethane, isocyanato, acrylate, glyceryl acrylate, benzyl-amino, vinyl-benzyl-amino.
  • the R 2 group may alter between any of the mentioned functional R 2 -groups and a hydrophobic alkyl group with repeatable units.
  • the metal-organic compound may be selected from derivates, intermediates or oligomers of silanes, siloxanes and silsesquioxanes or the corresponding titanates, aluminates or zirconates.
  • the metal-organic layer located outside the first layer is of a monomer of the metal-organic compound and wherein the outermost metal-organic layer is of an oligomer of the metal-organic compound.
  • the chemical functionality of the monomer and the oligomer is necessary not same.
  • the ratio by weight of the layer of the monomer of the metal-organic compound and the layer of the oligomer of the metal-organic compound may be between 1:0 and 1:2, preferably between 2:1-1:2.
  • the metal-organic compound is a monomer it may be selected from the group of trialkoxy and dialkoxy silanes, titanates, aluminates, or zirconates.
  • the monomer of the metal-organic compound may thus be selected from 3-aminopropyl-trimethoxysilane, 3-aminopropyl-triethoxysilane, 3-aminopropyl-methyldiethoxysilane, N-aminoethyl-3-aminopropyl-trimethoxysilane, N-aminoethyl-3-aminopropyl-methyl-dimethoxysilane, 1,7-bis(triethoxysilyl)-4-azaheptan, triamino-functional propyl-trimethoxysilane, 3-ureidopropyl-triethoxysilane, 3-isocyanatopropyl-triethoxysilane, tris(3-trimethoxysilylpropyl)-is
  • An oligomer of the metal-organic compound may be selected from alkoxy-terminated alkyl-alkoxy-oligomers of silanes, titantes, aluminates, or zirconates.
  • the oligomer of the metal-organic compound may thus be selected from methoxy, ethoxy or acetoxy-terminated amino-silsesquioxanes, amino-siloxanes, oligomeric 3-aminopropyl-methoxy-silane, 3-aminopropyl/propyl-alkoxy-silanes, N-aminoethyl-3-aminopropyl-alkoxy-silanes, or N-aminoethyl-3-aminopropyl/methyl-alkoxy-silanes or mixtures thereof.
  • the total amount of metal-organic compound may be 0.05-0.6 %, preferably 0.05-0.5 %, more preferably 0.1-0.4%, and most preferably 0.2-0.3% by weight of the composition.
  • These kinds of metal-organic compounds may be commercially obtained from companies, such as Evonik Ind., Wacker Chemie AG, Dow Corning, etc.
  • the metal-organic compound has an alkaline character and may also include coupling properties i.e. a so called coupling agent which will couple to the first inorganic layer of the iron-based powder.
  • the substance should neutralise the excess acids and acidic bi-products from the first layer. If coupling agents from the group of aminoalkyl alkoxy-silanes, -titanates, -aluminates, or -zirconates are used, the substance will hydrolyse and partly polymerise (some of the alkoxy groups will be hydrolysed with the formation of alcohol accordingly).
  • the coupling or cross-linking properties of the metal-organic compounds is also believed to couple to the metallic or semi-metallic particulate compound which may improve the mechanical stability of the compacted composite component.
  • the coated soft magnetic iron-based powder may also contain at least one metallic or semi-metallic particulate compound.
  • the metallic or semi-metallic particulate compound should be soft, having Mohs hardness less than 3.5, and constitute fine particles or colloids.
  • the compound may preferably have an average particle size below 5 ⁇ m, preferably below 3 ⁇ m, and most preferably below 1 ⁇ m.
  • the metallic or semi-metallic particulate compound may have a purity of more than 95%, preferably more than 98%, and most preferably more than 99% by weight.
  • the Mohs hardness of the metallic or semi-metallic particulate compound is preferably 3 or less, more preferably 2.5 or less.
  • SiO 2 , Al 2 O 3 , MgO, and TiO 2 are abrasive and have a Mohs hardness well above 3.5 and is not within the scope of the invention.
  • the metallic or semi-metallic particulate compound may be at least one selected from the group: lead, indium, bismuth, selenium, boron, molybdenum, manganese, tungsten, vanadium, antimony, tin, zinc, cerium.
  • the metallic or semi-metallic particulate compound may be an oxide, hydroxide, hydrate, carbonate, phosphate, fluorite, sulphide, sulphate, sulphite, oxychloride, or a mixture thereof.
  • the metallic or semi-metallic particulate compound is bismuth, or more preferably bismuth (III) oxide.
  • the metallic or semi-metallic particulate compound may be mixed with a second compound selected from alkaline or alkaline earth metals, wherein the compound may be carbonates, preferably carbonates of calcium, strontium, barium, lithium, potassium or sodium.
  • the metallic or semi-metallic particulate compound or compound mixture may be present in an amount of 0.05-0.5 %, preferably 0.1-0.4%, and most preferably 0.15-0.3% by weight of the composition.
  • the metallic or semi-metallic particulate compound is adhered to at least one metal-organic layer. In one embodiment of the invention the metallic or semi-metallic particulate compound is adhered to the outermost metal-organic layer.
  • the metal-organic layer may be formed by mixing the powder by stirring with different amounts of first a basic aminoalkyl-alkoxy silane (Dynasylan®Ameo) and thereafter with an oligomer of an aminoalkyl/alkyl-alkoxy silane (Dynasylan®1146), e.g. by using a 1:1 relation, both produced by Evonik Inc.
  • the composition may be further mixed with different amounts of a fine powder of bismuth(III) oxide (>99wt%; D 50 ⁇ 0.3 ⁇ m).
  • This good saturation flux density achieved by the material according to the invention makes it possible to downsize inductor components and still maintain good magnetic properties.
  • the coated iron-based composition may be mixed with a suitable organic lubricant such as a wax, an oligomer or a polymer, a fatty acid based derivate or combinations thereof.
  • suitable lubricants are EBS, i.e. ethylene bisstearamide, Kenolube® available from Höganäs AB, Sweden, metal stearates such as zinc stearate or fatty acids or other derivates thereof.
  • the lubricant may be added in an amount of 0.05-1.5% of the total mixture, preferably between 0.1-1.2% by weight.
  • Compaction may be performed at a compaction pressure of 400-1200 MPa at ambient or elevated temperature.
  • the compacted components are subjected to heat treatment at a temperature up to 800°C, preferably between 600-750 °C.
  • suitable atmospheres at heat treatment are inert atmosphere such as nitrogen or argon or oxidizing atmospheres such as air.
  • the powder magnetic core of the present invention is obtained by pressure forming an iron-based magnetic powder covered with a new electrically insulating coating.
  • the core may be characterized by low total losses in the frequency range 2-100 kHz, normally 5-100 kHz, of about less than 12W/kg at a frequency of 20kHz and induction of 0.05T.
  • a resisitivity, p more than 1000, preferably more than 2000 and most preferably more than 3000 ⁇ m, and a saturation magnetic flux density Bs above 1.1, preferably above 1.2 and most preferably above 1.3T.Further, the coersivity shall be below 210A/m, preferably below 200A/m, most preferably below 190A/m and DC- bias not less than 50% at 4000A/m.
  • the core particles have been mixed with grinded Sendust (typically 85%Fe, 9,5%Si and 5,5%Al) and the powder mix was then treated with a phosphorous containing solution according to WO2008/069749 . Briefly, the coating solution was prepared by dissolving 30 ml of 85 % weight of phosphoric acid in 1 000 ml of acetone, and 40 ml - 60 ml of acetone solution was used per 1000 gram of powder. After mixing the phosphoric acid solution with the metal powder, the mixture is allowed to dry.
  • grinded Sendust typically 85%Fe, 9,5%Si and 5,5%Al
  • the obtained dry phosphorous coated iron - sendust mix powder was further blended with kaolin and sodium silicate according to the following table 1. After drying at 120°C the powder was mixed with 0.6% Kenolube® and compacted at 800MPa into rings with an inner diameter of 45mm, an outer diameter of 55mm and a height of 5mm. The compacted components were thereafter subjected to a heat treatment process at 700°C in a nitrogen atmosphere for 0.5 hours.
  • the specific resistivities of the obtained samples were measured by a four point measurement.
  • the rings were "wired” with 100 turns for the primary circuit and 100 turns for the secondary circuit enabling measurements of magnetic properties with the aid of a hysteresisgraph, Brockhaus MPG 100.
  • the rings were "wired” with 30 turns for the primary circuit and 30 turns for the secondary circuit with the aid of Walker Scientific Inc. AMH-401 POD instrument.
  • This example shows that the phosphorous- clay- silicate coating concept according to the invention may be applied to different particle sizes of the iron powder - the Sendust powder has a fixed particle size of approximately 45 ⁇ m.
  • an iron powder having a mean particle size of ⁇ 45 ⁇ m has been used
  • an iron powder having a mean particle size of ⁇ 100 ⁇ m has been used
  • for sample X an iron powder having a mean particle size of ⁇ 210 ⁇ m has been used.
  • the iron - Sendust powder mix was coated with a first phosphorous containing layer. Thereafter some samples were further treated with 1% kaolin and 0.4% sodium silicate as earlier described. Heat treatment was performed for 0.5h at 700°C in nitrogen.
  • Table 4 shows that regardless of the particle size of the iron powder clear improvements of resistivity and core losses are obtained for components according to the present invention.
  • Example 5 illustrates that it is possible to use different types of water glass and different types of clays containing defined phyllosilicates.
  • the 60% atomized iron - 40% sendust powder mixes were coated as described above with the exception that various silicates (Na, K and Li) and various clays (kaolin and talc) containing phyllosilicates having electroneutral layers were used.
  • clays containing phyllosilicates having electrical charged layer Veegum® and a mica, were used.
  • Veegum® is a trade name of clay from the smectite group.
  • the mica used was muscovite.
  • the second layer in all the tests contained 1% of clay and 0.4wt-% of water glass. Heat treatment was perform-ed for 0.5h at 700°C in nitrogen.
  • Table 5 shows results from testing of the components.
  • Table 5 Sample Additives on the iron - Sendust mix Component properties
  • Type of clay Type of silicate Mol ratio silicate Resistivity [ ⁇ m] ⁇ max [-] Coercivity [A/m] Core loss at 0.05T 20kHz [W/kg] 60%Atomized iron + 40% Sendust - phosphorous coated with a second coating layer consisting of 1% clay and 0.4%silicate Y-e Y Inv Kaolin Na 2.5 72850 80 134 7.5 Z Inv Talc Na 2.5 72321 94 131 7.4 a Comp Veegum® Na 2.5 97 91 135 19.9 b Comp Mica Na 2.5 389 106 138 15.4 c Inv Kaolin Na 3.37 72569 84 136 7.3 d Inv Kaolin K 2.5 84992 86 140 8.4 e Inv Kaolin Li 2.5 77403 85 147 8.2
  • Example 6 illustrates that by varying the amounts of clay and alkaline silicate in the second layer the properties of the compacted and heat treated component can be controlled and optimized.
  • the samples were prepared and tested as described earlier. Heat treatment was performed for 0.5h at 700°C in nitrogen.
  • resistivity will decrease if the content of sodium silicate in the second layer exceeds 0.7% by weight. Resistivity will also decrease as the content of sodium silicate is decreased thus the content of silicate shall be between 0.2-0.7% by weight, preferably between 0.3-0,6 % by weight of the total 60%atomized iron - 40% Sendust powder mix. Further increased clay content in the second layer up to about 4% will increase resistivity but decrease core loss due to increased Coercivity. Thus, the upper limit of clay in the second layer is 5 %, preferably 4%, by weight of the iron- based composite powder. The lower limit for content of clay is 1%, preferably 3% as a too low content of clay will have a detrimental influence of resistivity and core loss.
  • the following example 7 illustrates that powder produced according to the invention can be compacted to different compaction pressures and at different compaction die temperatures.
  • the samples below have been treated as described above, 60%atomized iron and 40% Sendust has been phosphorous and clay - sodium silicate coated, the content of kaolin in the second layer was 2% and the content of sodium silicate was 0.4% by weight of the composite iron - Sendust powder.
  • Table 7 shows that high resistivity and low core losses are obtained for components, according to the invention, compacted to different compaction pressures and compacted at different compaction die temperatures. A rise of the density and a lowering of the losses can be observed when raising the compaction pressure from 400 to 800MPa, further increasing the compaction pressure however gives just little effect. The compaction die temperature only increases the resistivity slightly and does not give any further improvements of the magnetic properties.
  • the following example 8 illustrate that components produced from powder according to the invention can be heat treated in different atmospheres and different temperatures.
  • the samples below have been treated as described above, 60%atomized iron and 40% Sendust has been phosphorous- and clay - sodium silicate coated, the content of kaolin in the second layer was 2% and the content of sodium silicate was 0.4% by weight of the composite iron - Sendust powder.
  • Table 8 shows that high resistivity and low core losses are obtained for components according to the invention heat treated at between 650°C - 750°C in nitrogen atmosphere or in a mixed atmosphere with nitrogen and air.
  • the following example 9 illustrates that it is possible to boost the magnetic properties of components produced from powder according to the invention by adding gas atomized FeSi to the mix.
  • the iron - Sendust powder mixes have a first phosphorous coating layer and a second layer consisting of 2%kaolin and 0.4%sodium silicate.
  • the powder mixes have been compacted to 800MPa and heat treated at 700°C, for 30minutes in a nitrogen atmosphere.
  • a pure water atomized iron powder having a content of iron above 99.5% by weight has been used as core particles.
  • the mean particle size of the powder was about 45 ⁇ m.
  • the core particles have been mixed with Sendust (typically 85%Fe, 9%Si and 6%AI) and the powder mix was treated with a phosphorous containing solution according to WO2008/069749 .
  • the obtained dry phosphorous coated iron powder - sendust mix was further treated with a second (metal organic) coating layer as described in WO2009/116938 , namely mixing the powder by stirring with different amounts of first a basic aminoalkyl-alkoxy silane (Dynasylan®Ameo) and thereafter with an oligomer of an aminoalkyl/alkyl-alkoxy silane (Dynasylan®1146), using a 1:1 relation, both produced by Evonik Inc.
  • the composition was further mixed with different amounts of a fine powder of bismuth(III) oxide (>99wt%; D 50 ⁇ 0.3 ⁇ m).
  • the powder was mixed with 0.4% amide wax and compacted to 800 MPa into rings with an inner diameter of 45mm, an outer diameter of 55mm and a height of 5mm.
  • the compacted components were thereafter subjected to a heat treatment process at 700°C in a nitrogen atmosphere for 0.5 hours.
  • Samples Hh-Ii) were prepared according to table 10 which also shows results from testing of the components.
  • Table 10 Sample Additives on the iron - Sendust mix Heat treatment temperature Component properties Phosphorous coating Metal organic layer Resistivity [ ⁇ m] ⁇ max [-] Coercivity [A/m] Core loss at 0.05T 20kHz [W/kg] DC Bias [%] 100%Atomized Iron Hh Hh Comp Yes Yes 650 °C 19923 226 195 10,0 40 60%Atomized Iron + 40% Sendust Ii Ii Inv Yes Yes 700°C 125000 113 151 6.7 60

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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Claims (11)

  1. Composition de poudre à base de fer composite comprenant des particules de noyau, les particules de noyau étant un mélange de
    (a) particules d'alliage de fer essentiellement constituées de 7 % à 13 % en poids de silicium, 4 % à 7 % en poids d'aluminium, le reste étant constitué de fer, et
    (b) particules de fer atomisé,
    lesdites particules de noyau étant revêtues d'une première couche contenant du phosphore, et les particules de fer atomisé ayant une deuxième couche comprenant :
    (i) un silicate alcalin combiné à un minéral argileux contenant un phyllosilicate, sa couche tétraédrique de silicium-oxygène et ses couches octaédriques d'hydroxyde combinées étant électriquement neutres, ou ;
    (ii) une couche organique métallique.
  2. Poudre à base de fer composite selon la revendication 1, dans laquelle les particules d'alliage de fer sont une deuxième couche comprenant :
    a) un silicate alcalin combiné à un minéral argileux contenant un phyllosilicate, sa couche tétraédrique de silicium-oxygène et ses couches octaédriques d'hydroxyde combinées étant électriquement neutres, ou ;
    b) une couche organique métallique.
  3. Poudre à base de fer composite selon la revendication 2, dans laquelle les particules d'alliage de fer et les particules de fer atomisé ont la même deuxième couche.
  4. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 3, dans laquelle la deuxième couche comprend du kaolin et du silicate de sodium.
  5. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 4, comprenant en outre du FeSi atomisé.
  6. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 5, dans laquelle la couche contenant du phosphore présente une épaisseur comprise entre 20 et 300 nm.
  7. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 6, dans laquelle le revêtement phosphoreux est fourni par la mise en contact des particules de noyaux avec un composé phosphoreux dans un solvant, puis l'élimination du solvant par séchage.
  8. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 7, dans laquelle le composé phosphoreux est l'acide phosphorique ou le phosphate d'aluminium.
  9. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 8, dans laquelle la teneur en silicate alcalin est comprise entre 0,1 et 0,9 % en poids, de préférence entre 0,2 et 0,8 % en poids de la poudre à base de fer composite.
  10. Poudre à base de fer composite selon l'une quelconque des revendications 1 à 9, dans laquelle la teneur en argile est comprise entre 0,2 et 5 % en poids, de préférence entre 0,5 et 4 % en poids de la poudre à base de fer composite.
  11. Procédé de production d'un composant compacté et traité à la chaleur, comprenant les étapes consistant à :
    a) fournir une poudre à base de fer composite selon l'une quelconque des revendications 1 à 10,
    b) compacter la poudre à base de fer composite, éventuellement mélangée à un lubrifiant, dans un mouvement de presse uniaxial dans une filière à une pression de compactage comprise entre 400 et 1200 MPa,
    c) éjecter le composant compacté de la filière,
    d) traiter à la chaleur le composant éjecté dans une atmosphère non réductrice à une température allant jusqu'à 800 °C.
EP12713715.6A 2011-04-07 2012-04-05 Nouvelle composition de poudre composite à base de fer, et méthode de fabrication d'un composant de poudre Active EP2695171B1 (fr)

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JP2014515880A (ja) 2014-07-03
PL2695171T3 (pl) 2019-01-31
BR112013025814A2 (pt) 2018-05-02
CA2832005C (fr) 2019-11-26
RU2631246C2 (ru) 2017-09-20
WO2012136758A2 (fr) 2012-10-11
KR101884214B1 (ko) 2018-08-30
TW201303915A (zh) 2013-01-16
EP2695171A2 (fr) 2014-02-12
CN110085386A (zh) 2019-08-02
EP2509081A1 (fr) 2012-10-10
JP2017143259A (ja) 2017-08-17
KR20140034185A (ko) 2014-03-19
US20140049354A1 (en) 2014-02-20
RU2013149408A (ru) 2015-05-20
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